# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Tomoaki Tanase' _publ_contact_author_email TANASE@CC.NARA-WU.AC.JP _publ_section_title ; Interconversion between ladder-type octanuclear and linear tetranuclear copper(I) complexes supported by tetraphosphine ligands ; loop_ _publ_author_name 'Tomoaki Tanase' 'Takayuki Nakajima' 'Yukie Takemura' # Attachment 'tanase-revised3.cif' data__compound1a-revised2 #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731694' # CHEMICAL DATA _chemical_formula_sum 'C79.33 H78.67 Cl10.67 Cu8 O2 P8 ' _chemical_formula_moiety 'C79.33 H78.67 Cl10.67 Cu8 O2 P8 ' _chemical_formula_weight 2198.56 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 16.2006(5) _cell_length_b 20.6852(5) _cell_length_c 23.1478(2) _cell_angle_alpha 80.923(3) _cell_angle_beta 75.017(4) _cell_angle_gamma 87.930(5) _cell_volume 7399.5(3) _cell_formula_units_Z 3 _cell_measurement_reflns_used 14442 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312.12 _exptl_absorpt_coefficient_mu 2.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 0.725 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 70500 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 32744 _reflns_number_gt 22927 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1382 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 32744 _refine_ls_number_parameters 1458 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0861P)^2^+24.6167P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 1.38 _refine_diff_density_min -1.07 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu -0.22552(4) 0.38747(3) 0.60195(3) 0.03321(14) Uani 1.00 1 d . . . Cu(2) Cu -0.06205(4) 0.45526(3) 0.48504(3) 0.03216(14) Uani 1.00 1 d . . . Cu(3) Cu 0.12106(4) 0.50132(3) 0.38267(3) 0.03419(15) Uani 1.00 1 d . . . Cu(4) Cu 0.30981(5) 0.52655(3) 0.32041(4) 0.04393(18) Uani 1.00 1 d . . . Cu(5) Cu 0.31783(4) 0.13920(3) 0.41984(3) 0.03276(14) Uani 1.00 1 d . . . Cu(6) Cu 0.46869(4) 0.07872(3) 0.50000(3) 0.02852(14) Uani 1.00 1 d . . . Cu(7) Cu 0.57195(4) -0.00129(3) 0.59524(3) 0.03138(14) Uani 1.00 1 d . . . Cu(8) Cu 0.62475(4) -0.09905(3) 0.69077(3) 0.03237(14) Uani 1.00 1 d . . . Cu(9) Cu 0.19985(4) 0.15224(3) 0.79399(3) 0.03070(14) Uani 1.00 1 d . . . Cu(10) Cu 0.14606(4) 0.07105(3) 0.91732(3) 0.03283(14) Uani 1.00 1 d . . . Cu(11) Cu 0.04182(5) 0.00400(3) 1.05626(3) 0.03408(15) Uani 1.00 1 d . . . Cu(12) Cu -0.09523(5) -0.03819(3) 1.19611(3) 0.03548(15) Uani 1.00 1 d . . . Cl(1) Cl -0.37278(9) 0.39321(7) 0.65132(9) 0.0520(4) Uani 1.00 1 d . . . Cl(2) Cl -0.19915(8) 0.48805(6) 0.53815(6) 0.0298(2) Uani 1.00 1 d . . . Cl(3) Cl -0.00666(7) 0.55154(5) 0.42451(5) 0.0263(2) Uani 1.00 1 d . . . Cl(4) Cl 0.18849(9) 0.58239(6) 0.30075(6) 0.0374(2) Uani 1.00 1 d . . . Cl(5) Cl 0.29647(8) 0.19168(6) 0.32619(5) 0.0294(2) Uani 1.00 1 d . . . Cl(6) Cl 0.46717(7) 0.12472(6) 0.39974(5) 0.0264(2) Uani 1.00 1 d . . . Cl(7) Cl 0.60359(7) 0.03300(5) 0.49150(5) 0.0229(2) Uani 1.00 1 d . . . Cl(8) Cl 0.70894(7) -0.02476(6) 0.61065(5) 0.0283(2) Uani 1.00 1 d . . . Cl(9) Cl 0.13623(9) 0.12213(6) 0.72354(5) 0.0331(2) Uani 1.00 1 d . . . Cl(10) Cl 0.24520(8) 0.04987(6) 0.82878(5) 0.0290(2) Uani 1.00 1 d . . . Cl(11) Cl 0.11242(8) -0.03421(6) 0.96780(5) 0.0295(2) Uani 1.00 1 d . . . Cl(12) Cl -0.00296(8) -0.09239(6) 1.12257(5) 0.0296(2) Uani 1.00 1 d . . . Cl(21) Cl 0.7023(2) 0.51583(18) 0.3795(2) 0.1550(17) Uani 1.00 1 d . . . Cl(22) Cl 0.5761(3) 0.4303(2) 0.4666(2) 0.184(2) Uani 1.00 1 d . . . Cl(23) Cl 0.1421(2) 0.7638(2) 0.0290(2) 0.1517(15) Uani 1.00 1 d . . . Cl(24) Cl 0.2749(3) 0.8177(3) 0.0637(2) 0.185(2) Uani 1.00 1 d . . . P(1) P -0.16146(8) 0.29550(5) 0.58278(6) 0.0223(2) Uani 1.00 1 d . . . P(2) P -0.03169(8) 0.35649(5) 0.46464(5) 0.0217(2) Uani 1.00 1 d . . . P(3) P 0.13707(8) 0.39913(6) 0.36839(5) 0.0224(2) Uani 1.00 1 d . . . P(4) P 0.32767(8) 0.42529(6) 0.30529(6) 0.0285(2) Uani 1.00 1 d . . . P(5) P 0.23449(7) 0.14704(6) 0.50891(5) 0.0212(2) Uani 1.00 1 d . . . P(6) P 0.37702(7) 0.11130(5) 0.57700(5) 0.0207(2) Uani 1.00 1 d . . . P(7) P 0.47160(7) 0.03367(6) 0.66616(5) 0.0216(2) Uani 1.00 1 d . . . P(8) P 0.51707(8) -0.07314(6) 0.76180(5) 0.0242(2) Uani 1.00 1 d . . . P(9) P 0.18088(9) 0.24735(6) 0.82521(6) 0.0275(2) Uani 1.00 1 d . . . P(10) P 0.14226(8) 0.16420(6) 0.95130(5) 0.0245(2) Uani 1.00 1 d . . . P(11) P 0.05545(8) 0.09961(6) 1.08173(5) 0.0224(2) Uani 1.00 1 d . . . P(12) P -0.07412(8) 0.06250(6) 1.20572(5) 0.0233(2) Uani 1.00 1 d . . . O(1) O 0.4059(6) 0.7114(5) 0.1391(4) 0.065(2) Uiso 0.50 1 d P . . O(2) O 0.3219(8) 0.9387(6) 0.0005(6) 0.089(3) Uiso 0.50 1 d P . . O(3) O 0.3664(8) 0.6587(6) 0.1656(6) 0.089(3) Uiso 0.50 1 d P . . O(4) O 0.0410(10) 0.3620(8) 0.0353(7) 0.114(4) Uiso 0.50 1 d P . . O(5) O 0.2694(10) 0.6379(8) 0.1211(7) 0.115(4) Uiso 0.50 1 d P . . O(6) O 0.6067(16) 0.4388(12) 0.1201(11) 0.181(9) Uiso 0.50 1 d P . . C(1) C -0.0523(3) 0.2947(2) 0.5332(2) 0.0253(9) Uani 1.00 1 d . . . C(2) C 0.0822(3) 0.3389(2) 0.4331(2) 0.0263(9) Uani 1.00 1 d . . . C(3) C 0.2468(2) 0.3689(2) 0.3577(2) 0.0238(9) Uani 1.00 1 d . . . C(4) C 0.2660(2) 0.1017(2) 0.5745(2) 0.0220(8) Uani 1.00 1 d . . . C(5) C 0.3692(3) 0.0569(2) 0.6492(2) 0.0239(9) Uani 1.00 1 d . . . C(6) C 0.4326(3) -0.0286(2) 0.7325(2) 0.0244(9) Uani 1.00 1 d . . . C(7) C 0.1111(3) 0.2346(2) 0.9023(2) 0.0280(10) Uani 1.00 1 d . . . C(8) C 0.0582(3) 0.1692(2) 1.0207(2) 0.0273(10) Uani 1.00 1 d . . . C(9) C -0.0397(3) 0.1233(2) 1.1371(2) 0.0248(9) Uani 1.00 1 d . . . C(101) C -0.1519(3) 0.2415(2) 0.6509(2) 0.0254(9) Uani 1.00 1 d . . . C(102) C -0.2106(3) 0.2478(2) 0.7048(2) 0.0303(10) Uani 1.00 1 d . . . C(103) C -0.2060(4) 0.2107(2) 0.7585(2) 0.0428(13) Uani 1.00 1 d . . . C(104) C -0.1403(4) 0.1650(2) 0.7595(2) 0.0457(14) Uani 1.00 1 d . . . C(105) C -0.0809(3) 0.1581(2) 0.7054(3) 0.0427(14) Uani 1.00 1 d . . . C(106) C -0.0869(3) 0.1951(2) 0.6523(2) 0.0344(11) Uani 1.00 1 d . . . C(107) C -0.2218(2) 0.2499(2) 0.5458(2) 0.0230(9) Uani 1.00 1 d . . . C(108) C -0.2154(3) 0.1823(2) 0.5477(2) 0.0274(10) Uani 1.00 1 d . . . C(109) C -0.2601(3) 0.1519(2) 0.5156(2) 0.0329(11) Uani 1.00 1 d . . . C(110) C -0.3106(3) 0.1876(2) 0.4828(2) 0.0348(11) Uani 1.00 1 d . . . C(111) C -0.3176(3) 0.2549(2) 0.4812(2) 0.0321(11) Uani 1.00 1 d . . . C(112) C -0.2739(3) 0.2860(2) 0.5131(2) 0.0289(10) Uani 1.00 1 d . . . C(113) C -0.0849(3) 0.3274(2) 0.4135(2) 0.0301(10) Uani 1.00 1 d . . . C(114) C -0.0849(3) 0.2625(2) 0.4053(2) 0.0375(12) Uani 1.00 1 d . . . C(115) C -0.1261(4) 0.2438(3) 0.3658(3) 0.0555(19) Uani 1.00 1 d . . . C(116) C -0.1668(4) 0.2896(4) 0.3332(3) 0.067(2) Uani 1.00 1 d . . . C(117) C -0.1673(5) 0.3536(4) 0.3405(3) 0.077(2) Uani 1.00 1 d . . . C(118) C -0.1266(4) 0.3735(3) 0.3807(3) 0.0526(16) Uani 1.00 1 d . . . C(119) C 0.1034(3) 0.3797(2) 0.3044(2) 0.0293(10) Uani 1.00 1 d . . . C(120) C 0.1101(4) 0.3178(2) 0.2877(2) 0.0413(13) Uani 1.00 1 d . . . C(121) C 0.0814(4) 0.3055(3) 0.2396(3) 0.0547(17) Uani 1.00 1 d . . . C(122) C 0.0465(6) 0.3545(5) 0.2073(3) 0.083(2) Uani 1.00 1 d . . . C(123) C 0.0357(8) 0.4157(5) 0.2246(5) 0.107(3) Uani 1.00 1 d . . . C(124) C 0.0653(7) 0.4286(3) 0.2724(4) 0.081(2) Uani 1.00 1 d . . . C(125) C 0.3224(4) 0.4112(2) 0.2309(2) 0.0406(13) Uani 1.00 1 d . . . C(126) C 0.3388(5) 0.3533(3) 0.2107(2) 0.0541(17) Uani 1.00 1 d . . . C(127) C 0.3340(5) 0.3439(3) 0.1527(3) 0.0622(19) Uani 1.00 1 d . . . C(128) C 0.3122(7) 0.3922(5) 0.1163(4) 0.098(3) Uani 1.00 1 d . . . C(129) C 0.2694(8) 0.4443(6) 0.1426(5) 0.106(3) Uani 1.00 1 d . . . C(130) C 0.2853(7) 0.4564(5) 0.1960(4) 0.093(3) Uani 1.00 1 d . . . C(131) C 0.4287(3) 0.3898(2) 0.3144(2) 0.0391(12) Uani 1.00 1 d . . . C(132) C 0.4420(4) 0.3234(3) 0.3271(3) 0.0574(19) Uani 1.00 1 d . . . C(133) C 0.5219(4) 0.2999(3) 0.3322(4) 0.079(2) Uani 1.00 1 d . . . C(134) C 0.5867(5) 0.3413(5) 0.3237(6) 0.097(3) Uani 1.00 1 d . . . C(135) C 0.5757(5) 0.4096(5) 0.3067(7) 0.119(4) Uani 1.00 1 d . . . C(136) C 0.4959(5) 0.4326(4) 0.3032(5) 0.088(3) Uani 1.00 1 d . . . C(201) C 0.2180(3) 0.2290(2) 0.5281(2) 0.0239(9) Uani 1.00 1 d . . . C(202) C 0.1508(3) 0.2440(2) 0.5750(2) 0.0295(10) Uani 1.00 1 d . . . C(203) C 0.1417(3) 0.3069(2) 0.5903(2) 0.0367(12) Uani 1.00 1 d . . . C(204) C 0.2006(4) 0.3546(2) 0.5586(2) 0.0392(13) Uani 1.00 1 d . . . C(205) C 0.2683(3) 0.3410(2) 0.5128(2) 0.0388(12) Uani 1.00 1 d . . . C(206) C 0.2768(3) 0.2782(2) 0.4971(2) 0.0302(10) Uani 1.00 1 d . . . C(207) C 0.1269(3) 0.1158(2) 0.5194(2) 0.0243(9) Uani 1.00 1 d . . . C(208) C 0.0780(3) 0.0822(2) 0.5734(2) 0.0330(11) Uani 1.00 1 d . . . C(209) C -0.0027(3) 0.0582(2) 0.5775(2) 0.0392(12) Uani 1.00 1 d . . . C(210) C -0.0359(3) 0.0682(2) 0.5278(2) 0.0367(12) Uani 1.00 1 d . . . C(211) C 0.0120(3) 0.1021(2) 0.4731(2) 0.0359(12) Uani 1.00 1 d . . . C(212) C 0.0921(3) 0.1251(2) 0.4689(2) 0.0323(11) Uani 1.00 1 d . . . C(213) C 0.3878(3) 0.1933(2) 0.5932(2) 0.0251(9) Uani 1.00 1 d . . . C(214) C 0.3245(3) 0.2232(2) 0.6328(2) 0.0266(9) Uani 1.00 1 d . . . C(215) C 0.3378(3) 0.2866(2) 0.6430(2) 0.0363(11) Uani 1.00 1 d . . . C(216) C 0.4140(4) 0.3179(2) 0.6160(3) 0.0460(14) Uani 1.00 1 d . . . C(217) C 0.4774(4) 0.2883(3) 0.5779(3) 0.0543(17) Uani 1.00 1 d . . . C(218) C 0.4635(3) 0.2260(2) 0.5654(3) 0.0424(13) Uani 1.00 1 d . . . C(219) C 0.5032(2) 0.1034(2) 0.6947(2) 0.0242(9) Uani 1.00 1 d . . . C(220) C 0.4598(3) 0.1217(2) 0.7496(2) 0.0270(9) Uani 1.00 1 d . . . C(221) C 0.4869(3) 0.1746(2) 0.7694(2) 0.0363(11) Uani 1.00 1 d . . . C(222) C 0.5587(4) 0.2104(3) 0.7339(3) 0.0493(15) Uani 1.00 1 d . . . C(223) C 0.6002(4) 0.1938(3) 0.6792(3) 0.0520(16) Uani 1.00 1 d . . . C(224) C 0.5742(3) 0.1390(3) 0.6598(2) 0.0387(12) Uani 1.00 1 d . . . C(225) C 0.5468(3) -0.0187(2) 0.8080(2) 0.0298(10) Uani 1.00 1 d . . . C(226) C 0.4984(4) -0.0117(3) 0.8659(2) 0.0442(13) Uani 1.00 1 d . . . C(227) C 0.5242(5) 0.0326(4) 0.8970(3) 0.062(2) Uani 1.00 1 d . . . C(228) C 0.5945(5) 0.0712(4) 0.8710(4) 0.072(2) Uani 1.00 1 d . . . C(229) C 0.6414(4) 0.0654(3) 0.8136(4) 0.061(2) Uani 1.00 1 d . . . C(230) C 0.6182(3) 0.0195(2) 0.7824(2) 0.0407(12) Uani 1.00 1 d . . . C(231) C 0.4573(3) -0.1405(2) 0.8146(2) 0.0365(12) Uani 1.00 1 d . . . C(232) C 0.4949(4) -0.2006(3) 0.8190(3) 0.0559(17) Uani 1.00 1 d . . . C(233) C 0.4508(6) -0.2529(4) 0.8611(5) 0.093(3) Uani 1.00 1 d . . . C(234) C 0.3725(6) -0.2455(4) 0.8963(4) 0.092(3) Uani 1.00 1 d . . . C(235) C 0.3332(4) -0.1848(4) 0.8917(3) 0.068(2) Uani 1.00 1 d . . . C(236) C 0.3748(3) -0.1324(3) 0.8519(2) 0.0437(13) Uani 1.00 1 d . . . C(301) C 0.2679(3) 0.2998(2) 0.8265(2) 0.0343(11) Uani 1.00 1 d . . . C(302) C 0.2582(5) 0.3480(3) 0.8628(3) 0.0575(18) Uani 1.00 1 d . . . C(303) C 0.3236(5) 0.3920(3) 0.8566(3) 0.071(2) Uani 1.00 1 d . . . C(304) C 0.3981(5) 0.3884(3) 0.8141(4) 0.069(2) Uani 1.00 1 d . . . C(305) C 0.4109(4) 0.3406(3) 0.7780(3) 0.0608(18) Uani 1.00 1 d . . . C(306) C 0.3452(3) 0.2956(2) 0.7846(2) 0.0415(13) Uani 1.00 1 d . . . C(307) C 0.1164(3) 0.3034(2) 0.7849(2) 0.0336(11) Uani 1.00 1 d . . . C(308) C 0.1417(4) 0.3674(2) 0.7598(2) 0.0470(14) Uani 1.00 1 d . . . C(309) C 0.0895(4) 0.4062(3) 0.7301(3) 0.0532(16) Uani 1.00 1 d . . . C(310) C 0.0147(4) 0.3826(3) 0.7252(2) 0.0479(15) Uani 1.00 1 d . . . C(311) C -0.0103(4) 0.3188(3) 0.7485(3) 0.0503(15) Uani 1.00 1 d . . . C(312) C 0.0417(4) 0.2787(2) 0.7778(2) 0.0434(13) Uani 1.00 1 d . . . C(313) C 0.2414(3) 0.1920(2) 0.9635(2) 0.0295(10) Uani 1.00 1 d . . . C(314) C 0.2448(4) 0.2418(3) 0.9948(3) 0.0501(15) Uani 1.00 1 d . . . C(315) C 0.3233(5) 0.2640(4) 0.9995(3) 0.066(2) Uani 1.00 1 d . . . C(316) C 0.3972(4) 0.2329(4) 0.9732(3) 0.068(2) Uani 1.00 1 d . . . C(317) C 0.3946(4) 0.1836(4) 0.9427(3) 0.0578(18) Uani 1.00 1 d . . . C(318) C 0.3165(4) 0.1616(3) 0.9379(2) 0.0440(13) Uani 1.00 1 d . . . C(319) C 0.1480(3) 0.1153(2) 1.1084(2) 0.0276(10) Uani 1.00 1 d . . . C(320) C 0.1513(3) 0.1668(3) 1.1398(2) 0.0391(12) Uani 1.00 1 d . . . C(321) C 0.2255(4) 0.1769(3) 1.1567(3) 0.0506(15) Uani 1.00 1 d . . . C(322) C 0.2956(4) 0.1390(3) 1.1411(3) 0.0592(19) Uani 1.00 1 d . . . C(323) C 0.2936(4) 0.0897(3) 1.1098(3) 0.0583(18) Uani 1.00 1 d . . . C(324) C 0.2178(3) 0.0763(2) 1.0935(2) 0.0384(12) Uani 1.00 1 d . . . C(325) C 0.0069(3) 0.0695(2) 1.2460(2) 0.0261(9) Uani 1.00 1 d . . . C(326) C 0.0105(3) 0.1224(2) 1.2755(2) 0.0327(11) Uani 1.00 1 d . . . C(327) C 0.0750(4) 0.1267(3) 1.3039(2) 0.0480(15) Uani 1.00 1 d . . . C(328) C 0.1372(4) 0.0789(3) 1.3022(3) 0.0531(17) Uani 1.00 1 d . . . C(329) C 0.1343(3) 0.0263(3) 1.2730(3) 0.0481(15) Uani 1.00 1 d . . . C(330) C 0.0685(3) 0.0212(2) 1.2446(2) 0.0315(10) Uani 1.00 1 d . . . C(331) C -0.1663(3) 0.1019(2) 1.2499(2) 0.0298(10) Uani 1.00 1 d . . . C(332) C -0.2128(3) 0.1514(3) 1.2254(2) 0.0384(12) Uani 1.00 1 d . . . C(333) C -0.2846(3) 0.1772(3) 1.2609(3) 0.0483(15) Uani 1.00 1 d . . . C(334) C -0.3099(3) 0.1543(3) 1.3226(3) 0.0475(15) Uani 1.00 1 d . . . C(335) C -0.2645(4) 0.1046(2) 1.3472(2) 0.0445(14) Uani 1.00 1 d . . . C(336) C -0.1940(3) 0.0780(2) 1.3111(2) 0.0366(12) Uani 1.00 1 d . . . C(401) C 0.6355(10) 0.4967(8) 0.4578(8) 0.154(6) Uani 1.00 1 d . . . C(402) C 0.1793(11) 0.8139(11) 0.0671(8) 0.177(7) Uani 1.00 1 d . . . H(1) H -0.0129 0.3017 0.5556 0.031 Uiso 1.00 1 c R . . H(2) H -0.0424 0.2526 0.5207 0.031 Uiso 1.00 1 c R . . H(3) H 0.1112 0.3373 0.4644 0.032 Uiso 1.00 1 c R . . H(4) H 0.0863 0.2968 0.4204 0.032 Uiso 1.00 1 c R . . H(5) H 0.2596 0.3612 0.3962 0.029 Uiso 1.00 1 c R . . H(6) H 0.2499 0.3284 0.3425 0.029 Uiso 1.00 1 c R . . H(7) H 0.2300 0.1153 0.6098 0.027 Uiso 1.00 1 c R . . H(8) H 0.2564 0.0563 0.5752 0.027 Uiso 1.00 1 c R . . H(9) H 0.3356 0.0782 0.6809 0.030 Uiso 1.00 1 c R . . H(10) H 0.3400 0.0177 0.6481 0.030 Uiso 1.00 1 c R . . H(11) H 0.3966 -0.0082 0.7641 0.031 Uiso 1.00 1 c R . . H(12) H 0.3988 -0.0599 0.7219 0.031 Uiso 1.00 1 c R . . H(13) H 0.1123 0.2730 0.9201 0.035 Uiso 1.00 1 c R . . H(14) H 0.0540 0.2276 0.9002 0.035 Uiso 1.00 1 c R . . H(15) H 0.0666 0.2085 1.0355 0.034 Uiso 1.00 1 c R . . H(16) H 0.0042 0.1716 1.0112 0.034 Uiso 1.00 1 c R . . H(17) H -0.0272 0.1633 1.1488 0.030 Uiso 1.00 1 c R . . H(18) H -0.0853 0.1304 1.1181 0.030 Uiso 1.00 1 c R . . H(19) H -0.2560 0.2783 0.7047 0.037 Uiso 1.00 1 c R . . H(20) H -0.2476 0.2167 0.7951 0.054 Uiso 1.00 1 c R . . H(21) H -0.1370 0.1392 0.7969 0.055 Uiso 1.00 1 c R . . H(22) H -0.0353 0.1272 0.7051 0.052 Uiso 1.00 1 c R . . H(23) H -0.0457 0.1896 0.6155 0.042 Uiso 1.00 1 c R . . H(24) H -0.1810 0.1572 0.5709 0.034 Uiso 1.00 1 c R . . H(25) H -0.2556 0.1061 0.5155 0.039 Uiso 1.00 1 c R . . H(26) H -0.3410 0.1655 0.4615 0.043 Uiso 1.00 1 c R . . H(27) H -0.3530 0.2795 0.4585 0.039 Uiso 1.00 1 c R . . H(28) H -0.2791 0.3321 0.5128 0.035 Uiso 1.00 1 c R . . H(29) H -0.0554 0.2307 0.4270 0.046 Uiso 1.00 1 c R . . H(30) H -0.1270 0.1987 0.3614 0.067 Uiso 1.00 1 c R . . H(31) H -0.1939 0.2753 0.3053 0.080 Uiso 1.00 1 c R . . H(32) H -0.1975 0.3851 0.3180 0.094 Uiso 1.00 1 c R . . H(33) H -0.1272 0.4185 0.3868 0.063 Uiso 1.00 1 c R . . H(34) H 0.1341 0.2829 0.3107 0.050 Uiso 1.00 1 c R . . H(35) H 0.0877 0.2624 0.2283 0.065 Uiso 1.00 1 c R . . H(36) H 0.0265 0.3456 0.1740 0.098 Uiso 1.00 1 c R . . H(37) H 0.0159 0.4507 0.1989 0.139 Uiso 1.00 1 c R . . H(38) H 0.0535 0.4714 0.2858 0.101 Uiso 1.00 1 c R . . H(39) H 0.3557 0.3173 0.2366 0.065 Uiso 1.00 1 c R . . H(40) H 0.3488 0.3022 0.1387 0.076 Uiso 1.00 1 c R . . H(41) H 0.3166 0.3898 0.0749 0.181 Uiso 1.00 1 c R . . H(42) H 0.2377 0.4731 0.1207 0.227 Uiso 1.00 1 c R . . H(43) H 0.2668 0.4992 0.2083 0.167 Uiso 1.00 1 c R . . H(44) H 0.3954 0.2929 0.3317 0.070 Uiso 1.00 1 c R . . H(45) H 0.5315 0.2535 0.3398 0.095 Uiso 1.00 1 c R . . H(46) H 0.6402 0.3246 0.3308 0.112 Uiso 1.00 1 c R . . H(47) H 0.6233 0.4402 0.2952 0.125 Uiso 1.00 1 c R . . H(48) H 0.4859 0.4785 0.2956 0.102 Uiso 1.00 1 c R . . H(49) H 0.1100 0.2103 0.5970 0.037 Uiso 1.00 1 c R . . H(50) H 0.0955 0.3168 0.6230 0.045 Uiso 1.00 1 c R . . H(51) H 0.1941 0.3982 0.5684 0.046 Uiso 1.00 1 c R . . H(52) H 0.3235 0.2688 0.4644 0.037 Uiso 1.00 1 c R . . H(53) H 0.1005 0.0757 0.6080 0.040 Uiso 1.00 1 c R . . H(54) H -0.0357 0.0345 0.6152 0.047 Uiso 1.00 1 c R . . H(55) H -0.0913 0.0512 0.5300 0.044 Uiso 1.00 1 c R . . H(56) H -0.0111 0.1097 0.4386 0.043 Uiso 1.00 1 c R . . H(57) H 0.1249 0.1478 0.4312 0.040 Uiso 1.00 1 c R . . H(58) H 0.2718 0.2007 0.6529 0.032 Uiso 1.00 1 c R . . H(59) H 0.2938 0.3076 0.6693 0.044 Uiso 1.00 1 c R . . H(60) H 0.4223 0.3612 0.6229 0.055 Uiso 1.00 1 c R . . H(61) H 0.5315 0.3095 0.5610 0.066 Uiso 1.00 1 c R . . H(62) H 0.5066 0.2061 0.5367 0.051 Uiso 1.00 1 c R . . H(63) H 0.4107 0.0974 0.7738 0.033 Uiso 1.00 1 c R . . H(64) H 0.4559 0.1872 0.8069 0.043 Uiso 1.00 1 c R . . H(65) H 0.5792 0.2465 0.7478 0.061 Uiso 1.00 1 c R . . H(66) H 0.6473 0.2198 0.6536 0.061 Uiso 1.00 1 c R . . H(67) H 0.6057 0.1256 0.6226 0.047 Uiso 1.00 1 c R . . H(68) H 0.4474 -0.0375 0.8845 0.054 Uiso 1.00 1 c R . . H(69) H 0.4916 0.0377 0.9365 0.074 Uiso 1.00 1 c R . . H(70) H 0.6111 0.1014 0.8938 0.081 Uiso 1.00 1 c R . . H(71) H 0.6901 0.0933 0.7946 0.073 Uiso 1.00 1 c R . . H(72) H 0.6522 0.0144 0.7428 0.049 Uiso 1.00 1 c R . . H(73) H 0.5514 -0.2073 0.7929 0.069 Uiso 1.00 1 c R . . H(74) H 0.4780 -0.2955 0.8637 0.110 Uiso 1.00 1 c R . . H(75) H 0.3433 -0.2818 0.9241 0.108 Uiso 1.00 1 c R . . H(76) H 0.2763 -0.1792 0.9166 0.082 Uiso 1.00 1 c R . . H(77) H 0.3474 -0.0903 0.8495 0.053 Uiso 1.00 1 c R . . H(78) H 0.2060 0.3503 0.8934 0.071 Uiso 1.00 1 c R . . H(79) H 0.3150 0.4251 0.8823 0.083 Uiso 1.00 1 c R . . H(80) H 0.4434 0.4186 0.8109 0.083 Uiso 1.00 1 c R . . H(81) H 0.4639 0.3380 0.7473 0.074 Uiso 1.00 1 c R . . H(82) H 0.3539 0.2611 0.7601 0.050 Uiso 1.00 1 c R . . H(83) H 0.1952 0.3841 0.7629 0.057 Uiso 1.00 1 c R . . H(84) H 0.1062 0.4505 0.7118 0.063 Uiso 1.00 1 c R . . H(85) H -0.0213 0.4104 0.7050 0.058 Uiso 1.00 1 c R . . H(86) H -0.0640 0.3028 0.7457 0.061 Uiso 1.00 1 c R . . H(87) H 0.0267 0.2336 0.7920 0.053 Uiso 1.00 1 c R . . H(88) H 0.1920 0.2610 1.0147 0.062 Uiso 1.00 1 c R . . H(89) H 0.3254 0.3009 1.0201 0.081 Uiso 1.00 1 c R . . H(90) H 0.4507 0.2454 0.9779 0.084 Uiso 1.00 1 c R . . H(91) H 0.4466 0.1636 0.9232 0.071 Uiso 1.00 1 c R . . H(92) H 0.3150 0.1247 0.9175 0.054 Uiso 1.00 1 c R . . H(93) H 0.1034 0.1953 1.1494 0.047 Uiso 1.00 1 c R . . H(94) H 0.2265 0.2115 1.1803 0.061 Uiso 1.00 1 c R . . H(95) H 0.3468 0.1469 1.1528 0.072 Uiso 1.00 1 c R . . H(96) H 0.3439 0.0638 1.0981 0.069 Uiso 1.00 1 c R . . H(97) H 0.2159 0.0400 1.0725 0.048 Uiso 1.00 1 c R . . H(98) H -0.0321 0.1558 1.2766 0.039 Uiso 1.00 1 c R . . H(99) H 0.0762 0.1629 1.3249 0.058 Uiso 1.00 1 c R . . H(100) H 0.1824 0.0820 1.3213 0.064 Uiso 1.00 1 c R . . H(101) H 0.1774 -0.0069 1.2718 0.058 Uiso 1.00 1 c R . . H(102) H 0.0664 -0.0157 1.2240 0.039 Uiso 1.00 1 c R . . H(103) H -0.1945 0.1681 1.1830 0.046 Uiso 1.00 1 c R . . H(104) H -0.3175 0.2104 1.2428 0.059 Uiso 1.00 1 c R . . H(105) H -0.3577 0.1732 1.3480 0.056 Uiso 1.00 1 c R . . H(106) H -0.2825 0.0880 1.3897 0.054 Uiso 1.00 1 c R . . H(107) H -0.1629 0.0430 1.3290 0.045 Uiso 1.00 1 c R . . H(108) H 0.3098 0.3743 0.4918 0.048 Uiso 1.00 1 c R . . H(109) H 0.6727 0.4896 0.4861 0.185 Uiso 1.00 1 c R . . H(110) H 0.5979 0.5344 0.4678 0.185 Uiso 1.00 1 c R . . H(111) H 0.1610 0.8587 0.0539 0.213 Uiso 1.00 1 c R . . H(112) H 0.1492 0.8021 0.1104 0.213 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0339(3) 0.0202(2) 0.0433(3) 0.0029(2) -0.0032(2) -0.0098(2) Cu(2) 0.0370(3) 0.0189(2) 0.0385(3) -0.0006(2) -0.0042(2) -0.0072(2) Cu(3) 0.0340(3) 0.0199(2) 0.0454(3) -0.0004(2) -0.0013(2) -0.0100(2) Cu(4) 0.0450(4) 0.0222(3) 0.0540(4) -0.0053(2) 0.0103(3) -0.0115(2) Cu(5) 0.0303(3) 0.0416(3) 0.0239(3) 0.0064(2) -0.0021(2) -0.0072(2) Cu(6) 0.0258(3) 0.0291(3) 0.0293(3) 0.0037(2) -0.0025(2) -0.0089(2) Cu(7) 0.0294(3) 0.0382(3) 0.0250(3) 0.0115(2) -0.0043(2) -0.0073(2) Cu(8) 0.0323(3) 0.0349(3) 0.0295(3) 0.0107(2) -0.0065(2) -0.0086(2) Cu(9) 0.0365(3) 0.0267(3) 0.0268(3) -0.0040(2) -0.0027(2) -0.0058(2) Cu(10) 0.0422(3) 0.0265(3) 0.0278(3) -0.0040(2) -0.0029(2) -0.0075(2) Cu(11) 0.0451(4) 0.0262(3) 0.0291(3) -0.0056(2) -0.0032(2) -0.0081(2) Cu(12) 0.0467(4) 0.0271(3) 0.0304(3) -0.0098(2) -0.0032(2) -0.0069(2) Cl(1) 0.0288(7) 0.0355(7) 0.0858(11) -0.0069(5) 0.0053(7) -0.0233(7) Cl(2) 0.0271(6) 0.0236(5) 0.0374(6) 0.0029(4) -0.0073(5) -0.0032(4) Cl(3) 0.0281(5) 0.0193(4) 0.0301(5) 0.0016(4) -0.0058(4) -0.0026(4) Cl(4) 0.0465(7) 0.0236(5) 0.0363(6) -0.0047(5) 0.0001(5) -0.0038(4) Cl(5) 0.0347(6) 0.0231(5) 0.0302(6) 0.0069(4) -0.0098(5) -0.0027(4) Cl(6) 0.0230(5) 0.0277(5) 0.0264(5) -0.0003(4) -0.0033(4) -0.0029(4) Cl(7) 0.0217(5) 0.0221(5) 0.0241(5) -0.0007(4) -0.0045(4) -0.0037(4) Cl(8) 0.0249(5) 0.0272(5) 0.0328(6) 0.0027(4) -0.0092(4) -0.0027(4) Cl(9) 0.0404(7) 0.0358(6) 0.0205(5) -0.0069(5) -0.0042(5) -0.0015(4) Cl(10) 0.0248(5) 0.0306(5) 0.0285(5) -0.0009(4) -0.0002(4) -0.0056(4) Cl(11) 0.0364(6) 0.0253(5) 0.0242(5) -0.0019(4) -0.0023(4) -0.0047(4) Cl(12) 0.0354(6) 0.0260(5) 0.0243(5) -0.0011(4) -0.0025(4) -0.0035(4) Cl(21) 0.120(2) 0.091(2) 0.273(5) -0.0092(19) -0.063(3) -0.061(2) Cl(22) 0.219(5) 0.097(2) 0.239(5) -0.024(2) -0.089(4) 0.024(3) Cl(23) 0.095(2) 0.183(4) 0.163(3) 0.009(2) -0.021(2) -0.005(3) Cl(24) 0.212(5) 0.245(5) 0.114(2) -0.065(4) -0.057(3) -0.035(3) P(1) 0.0218(5) 0.0159(5) 0.0274(6) -0.0005(4) -0.0031(4) -0.0038(4) P(2) 0.0224(5) 0.0170(5) 0.0251(5) -0.0018(4) -0.0039(4) -0.0047(4) P(3) 0.0215(5) 0.0175(5) 0.0260(6) -0.0013(4) -0.0016(4) -0.0045(4) P(4) 0.0252(6) 0.0205(5) 0.0344(6) -0.0020(4) 0.0033(5) -0.0060(4) P(5) 0.0203(5) 0.0222(5) 0.0214(5) 0.0040(4) -0.0053(4) -0.0050(4) P(6) 0.0198(5) 0.0189(5) 0.0239(5) 0.0028(4) -0.0063(4) -0.0045(4) P(7) 0.0196(5) 0.0239(5) 0.0211(5) 0.0038(4) -0.0050(4) -0.0043(4) P(8) 0.0261(6) 0.0234(5) 0.0228(5) 0.0032(4) -0.0072(4) -0.0018(4) P(9) 0.0364(7) 0.0229(5) 0.0211(5) -0.0037(5) -0.0048(5) -0.0006(4) P(10) 0.0299(6) 0.0224(5) 0.0193(5) -0.0030(4) -0.0029(4) -0.0021(4) P(11) 0.0250(6) 0.0229(5) 0.0180(5) -0.0014(4) -0.0025(4) -0.0040(4) P(12) 0.0246(6) 0.0239(5) 0.0205(5) -0.0024(4) -0.0028(4) -0.0055(4) C(1) 0.024(2) 0.021(2) 0.030(2) -0.0018(17) -0.0043(19) -0.0037(18) C(2) 0.028(2) 0.022(2) 0.028(2) -0.0014(18) -0.007(2) -0.0027(18) C(3) 0.021(2) 0.022(2) 0.025(2) -0.0042(17) -0.0007(18) -0.0007(17) C(4) 0.020(2) 0.024(2) 0.022(2) 0.0021(17) -0.0049(17) -0.0036(17) C(5) 0.023(2) 0.024(2) 0.025(2) 0.0015(17) -0.0074(18) -0.0009(17) C(6) 0.026(2) 0.024(2) 0.025(2) 0.0077(18) -0.0091(19) -0.0061(17) C(7) 0.034(2) 0.027(2) 0.020(2) -0.001(2) -0.0030(19) 0.0006(18) C(8) 0.026(2) 0.029(2) 0.024(2) 0.0014(19) -0.0036(19) -0.0007(18) C(9) 0.026(2) 0.028(2) 0.020(2) 0.0003(18) -0.0046(18) -0.0050(18) C(101) 0.026(2) 0.019(2) 0.031(2) -0.0051(18) -0.010(2) -0.0010(18) C(102) 0.030(2) 0.023(2) 0.035(2) -0.0027(19) -0.004(2) -0.0035(19) C(103) 0.054(3) 0.036(2) 0.035(2) -0.016(2) -0.006(2) -0.001(2) C(104) 0.058(3) 0.036(3) 0.043(3) -0.010(2) -0.019(3) 0.010(2) C(105) 0.036(3) 0.030(2) 0.060(3) -0.003(2) -0.019(2) 0.010(2) C(106) 0.032(2) 0.028(2) 0.038(2) -0.002(2) -0.005(2) 0.005(2) C(107) 0.016(2) 0.018(2) 0.032(2) -0.0011(16) 0.0011(18) -0.0056(17) C(108) 0.023(2) 0.022(2) 0.034(2) -0.0032(18) -0.002(2) -0.0044(19) C(109) 0.031(2) 0.025(2) 0.038(2) -0.008(2) 0.002(2) -0.008(2) C(110) 0.028(2) 0.043(3) 0.034(2) -0.011(2) -0.001(2) -0.015(2) C(111) 0.026(2) 0.036(2) 0.035(2) -0.004(2) -0.008(2) -0.004(2) C(112) 0.023(2) 0.028(2) 0.033(2) -0.0045(19) -0.001(2) -0.005(2) C(113) 0.026(2) 0.033(2) 0.031(2) -0.008(2) -0.005(2) -0.006(2) C(114) 0.030(2) 0.040(2) 0.039(3) -0.007(2) 0.005(2) -0.019(2) C(115) 0.040(3) 0.076(4) 0.052(3) -0.024(3) 0.005(3) -0.040(3) C(116) 0.053(4) 0.106(6) 0.051(4) -0.032(4) -0.016(3) -0.023(4) C(117) 0.077(5) 0.095(6) 0.071(5) -0.028(4) -0.049(4) 0.004(4) C(118) 0.056(3) 0.047(3) 0.062(4) -0.011(3) -0.036(3) 0.007(3) C(119) 0.028(2) 0.028(2) 0.030(2) -0.0038(19) -0.005(2) -0.0039(19) C(120) 0.052(3) 0.037(2) 0.039(3) 0.004(2) -0.013(2) -0.018(2) C(121) 0.069(4) 0.061(4) 0.040(3) -0.017(3) -0.012(3) -0.021(3) C(122) 0.114(7) 0.095(6) 0.058(4) -0.015(5) -0.050(5) -0.018(4) C(123) 0.142(10) 0.092(7) 0.101(8) 0.013(7) -0.064(7) -0.001(6) C(124) 0.139(8) 0.048(4) 0.081(5) 0.018(4) -0.075(6) -0.008(3) C(125) 0.053(3) 0.030(2) 0.030(2) 0.004(2) 0.003(2) -0.003(2) C(126) 0.086(5) 0.036(3) 0.037(3) -0.010(3) -0.013(3) -0.000(2) C(127) 0.078(5) 0.062(4) 0.043(3) -0.012(3) 0.002(3) -0.022(3) C(128) 0.117(8) 0.090(7) 0.077(6) 0.018(6) -0.011(5) -0.007(5) C(129) 0.122(9) 0.098(8) 0.087(7) 0.015(7) -0.014(6) -0.009(6) C(130) 0.111(8) 0.083(6) 0.074(6) 0.016(5) -0.012(5) -0.006(5) C(131) 0.026(2) 0.038(2) 0.050(3) -0.005(2) -0.000(2) -0.013(2) C(132) 0.032(3) 0.035(3) 0.100(5) -0.003(2) -0.019(3) 0.007(3) C(133) 0.032(3) 0.049(4) 0.140(8) 0.005(3) -0.015(4) 0.022(4) C(134) 0.041(4) 0.081(6) 0.178(11) 0.007(4) -0.046(5) -0.017(6) C(135) 0.047(4) 0.082(6) 0.240(15) -0.005(4) -0.046(7) -0.046(8) C(136) 0.042(4) 0.049(4) 0.169(10) -0.003(3) -0.019(5) -0.019(5) C(201) 0.026(2) 0.020(2) 0.028(2) 0.0045(17) -0.0122(19) -0.0018(17) C(202) 0.026(2) 0.029(2) 0.036(2) 0.0047(19) -0.012(2) -0.006(2) C(203) 0.040(3) 0.035(2) 0.041(3) 0.017(2) -0.018(2) -0.015(2) C(204) 0.056(3) 0.020(2) 0.051(3) 0.011(2) -0.028(2) -0.011(2) C(205) 0.047(3) 0.027(2) 0.045(3) -0.004(2) -0.020(2) 0.003(2) C(206) 0.032(2) 0.028(2) 0.031(2) -0.003(2) -0.010(2) -0.0003(19) C(207) 0.024(2) 0.023(2) 0.027(2) 0.0032(18) -0.0046(19) -0.0100(18) C(208) 0.030(2) 0.033(2) 0.036(2) -0.001(2) -0.009(2) -0.005(2) C(209) 0.029(2) 0.044(3) 0.042(3) -0.003(2) -0.003(2) -0.008(2) C(210) 0.025(2) 0.029(2) 0.059(3) 0.002(2) -0.010(2) -0.015(2) C(211) 0.033(2) 0.034(2) 0.049(3) 0.005(2) -0.021(2) -0.013(2) C(212) 0.034(2) 0.031(2) 0.033(2) 0.003(2) -0.013(2) -0.006(2) C(213) 0.025(2) 0.021(2) 0.032(2) -0.0001(18) -0.011(2) -0.0050(18) C(214) 0.029(2) 0.025(2) 0.026(2) 0.0001(19) -0.007(2) -0.0056(18) C(215) 0.045(3) 0.028(2) 0.038(2) 0.005(2) -0.014(2) -0.009(2) C(216) 0.045(3) 0.024(2) 0.072(4) -0.003(2) -0.017(3) -0.012(2) C(217) 0.034(3) 0.031(2) 0.093(5) -0.012(2) 0.000(3) -0.019(3) C(218) 0.029(2) 0.032(2) 0.064(3) -0.001(2) 0.001(2) -0.019(2) C(219) 0.014(2) 0.031(2) 0.026(2) -0.0009(17) -0.0044(18) -0.0040(18) C(220) 0.023(2) 0.027(2) 0.030(2) -0.0014(18) -0.0026(19) -0.0072(19) C(221) 0.038(3) 0.033(2) 0.038(2) 0.002(2) -0.005(2) -0.012(2) C(222) 0.045(3) 0.051(3) 0.058(3) -0.013(2) -0.012(3) -0.024(3) C(223) 0.046(3) 0.057(3) 0.049(3) -0.032(3) 0.002(2) -0.011(3) C(224) 0.040(3) 0.047(3) 0.027(2) -0.015(2) -0.002(2) -0.010(2) C(225) 0.030(2) 0.031(2) 0.034(2) 0.005(2) -0.016(2) -0.010(2) C(226) 0.049(3) 0.046(3) 0.038(3) 0.003(2) -0.009(2) -0.015(2) C(227) 0.081(5) 0.072(4) 0.048(3) 0.016(4) -0.025(3) -0.038(3) C(228) 0.076(5) 0.070(5) 0.098(6) 0.014(4) -0.050(5) -0.056(4) C(229) 0.047(3) 0.043(3) 0.105(6) -0.002(2) -0.035(4) -0.023(3) C(230) 0.034(2) 0.040(3) 0.052(3) 0.001(2) -0.016(2) -0.011(2) C(231) 0.038(3) 0.037(2) 0.031(2) -0.007(2) -0.012(2) 0.012(2) C(232) 0.052(3) 0.036(3) 0.070(4) -0.002(2) -0.011(3) 0.014(3) C(233) 0.079(6) 0.051(4) 0.131(8) -0.009(4) -0.023(6) 0.041(5) C(234) 0.069(5) 0.082(6) 0.101(7) -0.026(4) -0.016(5) 0.053(5) C(235) 0.042(3) 0.094(6) 0.054(4) -0.019(3) -0.005(3) 0.023(4) C(236) 0.040(3) 0.052(3) 0.036(3) -0.009(2) -0.010(2) 0.007(2) C(301) 0.048(3) 0.028(2) 0.028(2) -0.007(2) -0.014(2) 0.002(2) C(302) 0.076(4) 0.045(3) 0.048(3) -0.023(3) -0.000(3) -0.017(2) C(303) 0.084(5) 0.059(4) 0.063(4) -0.039(4) 0.006(4) -0.020(3) C(304) 0.077(5) 0.049(4) 0.082(5) -0.031(3) -0.027(4) 0.001(3) C(305) 0.040(3) 0.061(4) 0.073(4) -0.009(3) -0.003(3) -0.001(3) C(306) 0.040(3) 0.040(3) 0.045(3) 0.002(2) -0.012(2) -0.005(2) C(307) 0.047(3) 0.024(2) 0.029(2) -0.002(2) -0.008(2) -0.0012(19) C(308) 0.055(3) 0.034(2) 0.047(3) -0.005(2) -0.013(2) 0.013(2) C(309) 0.061(4) 0.037(3) 0.054(3) -0.003(2) -0.012(3) 0.013(2) C(310) 0.057(4) 0.047(3) 0.038(3) 0.012(3) -0.017(2) 0.002(2) C(311) 0.061(4) 0.046(3) 0.052(3) 0.009(3) -0.028(3) -0.010(2) C(312) 0.057(3) 0.037(3) 0.040(3) -0.004(2) -0.022(2) -0.002(2) C(313) 0.033(2) 0.028(2) 0.024(2) -0.006(2) -0.004(2) 0.0031(19) C(314) 0.049(3) 0.051(3) 0.054(3) -0.008(2) -0.011(3) -0.019(3) C(315) 0.063(4) 0.078(5) 0.067(4) -0.025(4) -0.016(3) -0.031(4) C(316) 0.039(3) 0.105(6) 0.062(4) -0.025(4) -0.007(3) -0.022(4) C(317) 0.036(3) 0.086(5) 0.053(4) -0.006(3) -0.010(3) -0.016(3) C(318) 0.041(3) 0.057(3) 0.032(2) 0.000(2) -0.007(2) -0.006(2) C(319) 0.026(2) 0.028(2) 0.026(2) -0.0028(19) -0.0052(19) 0.0029(19) C(320) 0.034(2) 0.046(3) 0.040(3) -0.004(2) -0.011(2) -0.012(2) C(321) 0.047(3) 0.060(4) 0.050(3) -0.019(3) -0.020(3) -0.007(3) C(322) 0.042(3) 0.069(4) 0.070(4) -0.017(3) -0.030(3) 0.009(3) C(323) 0.036(3) 0.069(4) 0.066(4) 0.016(3) -0.017(3) 0.003(3) C(324) 0.029(2) 0.040(3) 0.040(3) 0.004(2) -0.005(2) 0.002(2) C(325) 0.030(2) 0.029(2) 0.017(2) -0.0068(19) -0.0032(19) 0.0021(17) C(326) 0.036(2) 0.036(2) 0.028(2) -0.005(2) -0.009(2) -0.009(2) C(327) 0.058(4) 0.060(3) 0.031(2) -0.019(3) -0.018(2) -0.008(2) C(328) 0.046(3) 0.070(4) 0.047(3) -0.021(3) -0.030(3) 0.018(3) C(329) 0.030(3) 0.058(3) 0.051(3) -0.002(2) -0.013(2) 0.011(3) C(330) 0.028(2) 0.035(2) 0.029(2) 0.001(2) -0.005(2) 0.000(2) C(331) 0.025(2) 0.036(2) 0.028(2) -0.005(2) -0.001(2) -0.012(2) C(332) 0.025(2) 0.055(3) 0.036(2) 0.003(2) -0.004(2) -0.015(2) C(333) 0.028(2) 0.056(3) 0.064(4) 0.010(2) -0.011(2) -0.025(3) C(334) 0.028(2) 0.055(3) 0.057(3) -0.009(2) 0.007(2) -0.033(3) C(335) 0.048(3) 0.037(3) 0.038(3) -0.019(2) 0.015(2) -0.013(2) C(336) 0.037(3) 0.031(2) 0.033(2) -0.005(2) 0.008(2) -0.006(2) C(401) 0.136(12) 0.149(13) 0.214(17) -0.034(10) -0.113(13) -0.019(11) C(402) 0.156(15) 0.24(2) 0.171(16) 0.033(14) -0.073(13) -0.097(15) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) Cu(4) 2.7968(10) yes . 2_566 Cu(1) Cl(1) 2.3716(14) yes . . Cu(1) Cl(2) 2.3368(13) yes . . Cu(1) P(1) 2.1860(12) yes . . Cu(2) Cl(2) 2.3764(13) yes . . Cu(2) Cl(3) 2.3094(11) yes . . Cu(2) P(2) 2.1796(12) yes . . Cu(3) Cl(2) 2.5208(17) yes . 2_566 Cu(3) Cl(3) 2.3290(12) yes . . Cu(3) Cl(4) 2.3789(12) yes . . Cu(3) P(3) 2.1866(14) yes . . Cu(4) Cl(1) 2.2437(19) yes . 2_566 Cu(4) Cl(4) 2.3531(16) yes . . Cu(4) P(4) 2.1745(14) yes . . Cu(5) Cu(8) 2.7376(9) yes . 2_656 Cu(5) Cl(5) 2.3698(13) yes . . Cu(5) Cl(6) 2.3599(12) yes . . Cu(5) P(5) 2.1796(12) yes . . Cu(6) Cl(6) 2.3713(13) yes . . Cu(6) Cl(7) 2.3230(12) yes . . Cu(6) Cl(7) 2.5852(12) yes . 2_656 Cu(6) P(6) 2.1851(12) yes . . Cu(7) Cl(7) 2.3205(12) yes . . Cu(7) Cl(8) 2.3591(13) yes . . Cu(7) P(7) 2.1842(12) yes . . Cu(8) Cl(5) 2.2926(13) yes . 2_656 Cu(8) Cl(8) 2.3676(11) yes . . Cu(8) P(8) 2.1820(12) yes . . Cu(9) Cl(9) 2.3120(16) yes . . Cu(9) Cl(10) 2.3082(13) yes . . Cu(9) P(9) 2.1857(14) yes . . Cu(10) Cl(10) 2.3457(12) yes . . Cu(10) Cl(11) 2.3145(12) yes . . Cu(10) P(10) 2.1863(14) yes . . Cu(11) Cl(11) 2.3152(13) yes . . Cu(11) Cl(12) 2.3283(12) yes . . Cu(11) P(11) 2.1851(14) yes . . Cu(12) Cl(9) 2.3110(12) yes . 2_557 Cu(12) Cl(12) 2.3568(13) yes . . Cu(12) P(12) 2.1775(14) yes . . Cl(21) C(401) 1.845(17) yes . . Cl(22) C(401) 1.663(17) yes . . Cl(23) C(402) 1.68(2) yes . . Cl(24) C(402) 1.53(2) yes . . P(1) C(1) 1.844(4) yes . . P(1) C(101) 1.821(4) yes . . P(1) C(107) 1.825(5) yes . . P(2) C(1) 1.838(4) yes . . P(2) C(2) 1.846(4) yes . . P(2) C(113) 1.816(6) yes . . P(3) C(2) 1.842(4) yes . . P(3) C(3) 1.831(4) yes . . P(3) C(119) 1.810(6) yes . . P(4) C(3) 1.842(4) yes . . P(4) C(125) 1.815(6) yes . . P(4) C(131) 1.818(6) yes . . P(5) C(4) 1.833(4) yes . . P(5) C(201) 1.812(4) yes . . P(5) C(207) 1.825(5) yes . . P(6) C(4) 1.833(5) yes . . P(6) C(5) 1.838(4) yes . . P(6) C(213) 1.818(5) yes . . P(7) C(5) 1.833(5) yes . . P(7) C(6) 1.830(4) yes . . P(7) C(219) 1.818(5) yes . . P(8) C(6) 1.836(5) yes . . P(8) C(225) 1.824(6) yes . . P(8) C(231) 1.822(5) yes . . P(9) C(7) 1.833(4) yes . . P(9) C(301) 1.818(6) yes . . P(9) C(307) 1.839(5) yes . . P(10) C(7) 1.840(5) yes . . P(10) C(8) 1.832(4) yes . . P(10) C(313) 1.827(5) yes . . P(11) C(8) 1.844(4) yes . . P(11) C(9) 1.839(4) yes . . P(11) C(319) 1.820(5) yes . . P(12) C(9) 1.838(4) yes . . P(12) C(325) 1.818(5) yes . . P(12) C(331) 1.824(5) yes . . O(1) O(3) 1.270(16) yes . . C(101) C(102) 1.382(6) yes . . C(101) C(106) 1.402(7) yes . . C(102) C(103) 1.372(7) yes . . C(103) C(104) 1.399(9) yes . . C(104) C(105) 1.392(8) yes . . C(105) C(106) 1.366(8) yes . . C(107) C(108) 1.392(6) yes . . C(107) C(112) 1.397(7) yes . . C(108) C(109) 1.391(8) yes . . C(109) C(110) 1.374(8) yes . . C(110) C(111) 1.388(7) yes . . C(111) C(112) 1.384(8) yes . . C(113) C(114) 1.384(8) yes . . C(113) C(118) 1.390(9) yes . . C(114) C(115) 1.369(10) yes . . C(115) C(116) 1.374(11) yes . . C(116) C(117) 1.360(14) yes . . C(117) C(118) 1.390(13) yes . . C(119) C(120) 1.387(8) yes . . C(119) C(124) 1.381(10) yes . . C(120) C(121) 1.373(10) yes . . C(121) C(122) 1.358(12) yes . . C(122) C(123) 1.379(16) yes . . C(123) C(124) 1.379(18) yes . . C(125) C(126) 1.347(8) yes . . C(125) C(130) 1.363(12) yes . . C(126) C(127) 1.411(10) yes . . C(127) C(128) 1.302(13) yes . . C(128) C(129) 1.395(17) yes . . C(129) C(130) 1.388(18) yes . . C(131) C(132) 1.379(8) yes . . C(131) C(136) 1.374(10) yes . . C(132) C(133) 1.393(10) yes . . C(133) C(134) 1.333(12) yes . . C(134) C(135) 1.423(15) yes . . C(135) C(136) 1.381(13) yes . . C(201) C(202) 1.389(6) yes . . C(201) C(206) 1.396(6) yes . . C(202) C(203) 1.396(7) yes . . C(203) C(204) 1.378(7) yes . . C(204) C(205) 1.369(7) yes . . C(205) C(206) 1.396(7) yes . . C(207) C(208) 1.389(6) yes . . C(207) C(212) 1.407(8) yes . . C(208) C(209) 1.391(8) yes . . C(209) C(210) 1.376(9) yes . . C(210) C(211) 1.395(7) yes . . C(211) C(212) 1.373(8) yes . . C(213) C(214) 1.386(6) yes . . C(213) C(218) 1.376(6) yes . . C(214) C(215) 1.403(7) yes . . C(215) C(216) 1.365(8) yes . . C(216) C(217) 1.365(9) yes . . C(217) C(218) 1.402(9) yes . . C(219) C(220) 1.387(6) yes . . C(219) C(224) 1.382(6) yes . . C(220) C(221) 1.378(8) yes . . C(221) C(222) 1.398(7) yes . . C(222) C(223) 1.361(9) yes . . C(223) C(224) 1.398(10) yes . . C(225) C(226) 1.394(7) yes . . C(225) C(230) 1.371(7) yes . . C(226) C(227) 1.387(11) yes . . C(227) C(228) 1.362(11) yes . . C(228) C(229) 1.371(12) yes . . C(229) C(230) 1.395(11) yes . . C(231) C(232) 1.366(8) yes . . C(231) C(236) 1.413(7) yes . . C(232) C(233) 1.412(10) yes . . C(233) C(234) 1.337(13) yes . . C(234) C(235) 1.387(13) yes . . C(235) C(236) 1.376(9) yes . . C(301) C(302) 1.382(9) yes . . C(301) C(306) 1.380(7) yes . . C(302) C(303) 1.386(12) yes . . C(303) C(304) 1.354(11) yes . . C(304) C(305) 1.369(12) yes . . C(305) C(306) 1.404(10) yes . . C(307) C(308) 1.389(7) yes . . C(307) C(312) 1.388(9) yes . . C(308) C(309) 1.384(10) yes . . C(309) C(310) 1.360(10) yes . . C(310) C(311) 1.376(8) yes . . C(311) C(312) 1.388(9) yes . . C(313) C(314) 1.361(9) yes . . C(313) C(318) 1.384(7) yes . . C(314) C(315) 1.403(11) yes . . C(315) C(316) 1.382(11) yes . . C(316) C(317) 1.337(13) yes . . C(317) C(318) 1.396(10) yes . . C(319) C(320) 1.390(8) yes . . C(319) C(324) 1.367(7) yes . . C(320) C(321) 1.389(10) yes . . C(321) C(322) 1.359(9) yes . . C(322) C(323) 1.347(12) yes . . C(323) C(324) 1.422(10) yes . . C(325) C(326) 1.387(7) yes . . C(325) C(330) 1.385(7) yes . . C(326) C(327) 1.384(9) yes . . C(327) C(328) 1.384(9) yes . . C(328) C(329) 1.376(11) yes . . C(329) C(330) 1.404(9) yes . . C(331) C(332) 1.386(8) yes . . C(331) C(336) 1.386(7) yes . . C(332) C(333) 1.383(8) yes . . C(333) C(334) 1.389(9) yes . . C(334) C(335) 1.377(9) yes . . C(335) C(336) 1.384(7) yes . . C(1) H(1) 0.949 no . . C(1) H(2) 0.956 no . . C(2) H(3) 0.956 no . . C(2) H(4) 0.956 no . . C(3) H(5) 0.955 no . . C(3) H(6) 0.953 no . . C(4) H(7) 0.950 no . . C(4) H(8) 0.954 no . . C(5) H(9) 0.952 no . . C(5) H(10) 0.959 no . . C(6) H(11) 0.955 no . . C(6) H(12) 0.961 no . . C(7) H(13) 0.953 no . . C(7) H(14) 0.955 no . . C(8) H(15) 0.958 no . . C(8) H(16) 0.953 no . . C(9) H(17) 0.955 no . . C(9) H(18) 0.951 no . . C(102) H(19) 0.952 no . . C(103) H(20) 0.957 no . . C(104) H(21) 0.957 no . . C(105) H(22) 0.958 no . . C(106) H(23) 0.957 no . . C(108) H(24) 0.955 no . . C(109) H(25) 0.947 no . . C(110) H(26) 0.953 no . . C(111) H(27) 0.957 no . . C(112) H(28) 0.953 no . . C(114) H(29) 0.956 no . . C(115) H(30) 0.955 no . . C(116) H(31) 0.956 no . . C(117) H(32) 0.968 no . . C(118) H(33) 0.963 no . . C(120) H(34) 0.961 no . . C(121) H(35) 0.963 no . . C(122) H(36) 0.955 no . . C(123) H(37) 0.962 no . . C(124) H(38) 0.980 no . . C(126) H(39) 0.957 no . . C(127) H(40) 0.968 no . . C(128) H(41) 0.952 no . . C(129) H(42) 0.944 no . . C(130) H(43) 0.986 no . . C(132) H(44) 0.976 no . . C(133) H(45) 0.963 no . . C(134) H(46) 0.966 no . . C(135) H(47) 0.971 no . . C(136) H(48) 0.953 no . . C(202) H(49) 0.963 no . . C(203) H(50) 0.958 no . . C(204) H(51) 0.960 no . . C(205) H(108) 0.960 no . . C(206) H(52) 0.959 no . . C(208) H(53) 0.952 no . . C(209) H(54) 0.964 no . . C(210) H(55) 0.961 no . . C(211) H(56) 0.957 no . . C(212) H(57) 0.956 no . . C(214) H(58) 0.956 no . . C(215) H(59) 0.952 no . . C(216) H(60) 0.955 no . . C(217) H(61) 0.954 no . . C(218) H(62) 0.961 no . . C(220) H(63) 0.953 no . . C(221) H(64) 0.953 no . . C(222) H(65) 0.958 no . . C(223) H(66) 0.960 no . . C(224) H(67) 0.959 no . . C(226) H(68) 0.963 no . . C(227) H(69) 0.952 no . . C(228) H(70) 0.964 no . . C(229) H(71) 0.960 no . . C(230) H(72) 0.958 no . . C(232) H(73) 0.976 no . . C(233) H(74) 0.970 no . . C(234) H(75) 0.958 no . . C(235) H(76) 0.967 no . . C(236) H(77) 0.963 no . . C(302) H(78) 0.958 no . . C(303) H(79) 0.961 no . . C(304) H(80) 0.962 no . . C(305) H(81) 0.969 no . . C(306) H(82) 0.965 no . . C(308) H(83) 0.968 no . . C(309) H(84) 0.962 no . . C(310) H(85) 0.960 no . . C(311) H(86) 0.964 no . . C(312) H(87) 0.957 no . . C(314) H(88) 0.964 no . . C(315) H(89) 0.967 no . . C(316) H(90) 0.951 no . . C(317) H(91) 0.960 no . . C(318) H(92) 0.964 no . . C(320) H(93) 0.960 no . . C(321) H(94) 0.969 no . . C(322) H(95) 0.964 no . . C(323) H(96) 0.961 no . . C(324) H(97) 0.964 no . . C(326) H(98) 0.957 no . . C(327) H(99) 0.958 no . . C(328) H(100) 0.957 no . . C(329) H(101) 0.961 no . . C(330) H(102) 0.967 no . . C(332) H(103) 0.959 no . . C(333) H(104) 0.965 no . . C(334) H(105) 0.956 no . . C(335) H(106) 0.961 no . . C(336) H(107) 0.968 no . . C(401) H(109) 0.990 no . . C(401) H(110) 0.990 no . . C(402) H(111) 0.990 no . . C(402) H(112) 0.990 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(4) Cu(1) Cl(1) 50.64(4) yes 2_566 . . Cu(4) Cu(1) Cl(2) 78.68(3) yes 2_566 . . Cu(4) Cu(1) P(1) 153.32(4) yes 2_566 . . Cl(1) Cu(1) Cl(2) 103.07(5) yes . . . Cl(1) Cu(1) P(1) 122.84(5) yes . . . Cl(2) Cu(1) P(1) 125.39(4) yes . . . Cl(2) Cu(2) Cl(3) 102.38(4) yes . . . Cl(2) Cu(2) P(2) 124.08(5) yes . . . Cl(3) Cu(2) P(2) 126.32(4) yes . . . Cl(2) Cu(3) Cl(3) 98.94(4) yes 2_566 . . Cl(2) Cu(3) Cl(4) 102.75(5) yes 2_566 . . Cl(2) Cu(3) P(3) 105.20(5) yes 2_566 . . Cl(3) Cu(3) Cl(4) 102.57(4) yes . . . Cl(3) Cu(3) P(3) 126.38(5) yes . . . Cl(4) Cu(3) P(3) 117.20(4) yes . . . Cu(1) Cu(4) Cl(1) 54.81(4) yes 2_566 . 2_566 Cu(1) Cu(4) Cl(4) 61.06(4) yes 2_566 . . Cu(1) Cu(4) P(4) 146.33(4) yes 2_566 . . Cl(1) Cu(4) Cl(4) 99.96(5) yes 2_566 . . Cl(1) Cu(4) P(4) 141.56(6) yes 2_566 . . Cl(4) Cu(4) P(4) 118.45(6) yes . . . Cu(8) Cu(5) Cl(5) 52.75(3) yes 2_656 . . Cu(8) Cu(5) Cl(6) 71.25(3) yes 2_656 . . Cu(8) Cu(5) P(5) 158.98(4) yes 2_656 . . Cl(5) Cu(5) Cl(6) 103.93(4) yes . . . Cl(5) Cu(5) P(5) 125.66(5) yes . . . Cl(6) Cu(5) P(5) 124.36(5) yes . . . Cl(6) Cu(6) Cl(7) 104.88(4) yes . . . Cl(6) Cu(6) Cl(7) 100.22(4) yes . . 2_656 Cl(6) Cu(6) P(6) 120.24(4) yes . . . Cl(7) Cu(6) Cl(7) 93.26(4) yes . . 2_656 Cl(7) Cu(6) P(6) 131.06(5) yes . . . Cl(7) Cu(6) P(6) 96.26(4) yes 2_656 . . Cl(7) Cu(7) Cl(8) 101.83(4) yes . . . Cl(7) Cu(7) P(7) 128.49(5) yes . . . Cl(8) Cu(7) P(7) 120.05(5) yes . . . Cu(5) Cu(8) Cl(5) 55.36(3) yes 2_656 . 2_656 Cu(5) Cu(8) Cl(8) 62.18(3) yes 2_656 . . Cu(5) Cu(8) P(8) 148.42(5) yes 2_656 . . Cl(5) Cu(8) Cl(8) 98.31(4) yes 2_656 . . Cl(5) Cu(8) P(8) 135.44(4) yes 2_656 . . Cl(8) Cu(8) P(8) 125.74(5) yes . . . Cl(9) Cu(9) Cl(10) 98.06(5) yes . . . Cl(9) Cu(9) P(9) 123.56(5) yes . . . Cl(10) Cu(9) P(9) 136.38(6) yes . . . Cl(10) Cu(10) Cl(11) 101.01(4) yes . . . Cl(10) Cu(10) P(10) 122.57(4) yes . . . Cl(11) Cu(10) P(10) 131.01(5) yes . . . Cl(11) Cu(11) Cl(12) 102.51(4) yes . . . Cl(11) Cu(11) P(11) 127.75(4) yes . . . Cl(12) Cu(11) P(11) 126.08(5) yes . . . Cl(9) Cu(12) Cl(12) 101.98(4) yes 2_557 . . Cl(9) Cu(12) P(12) 124.15(5) yes 2_557 . . Cl(12) Cu(12) P(12) 122.63(5) yes . . . Cu(1) Cl(1) Cu(4) 74.54(5) yes . . 2_566 Cu(1) Cl(2) Cu(2) 92.89(4) yes . . . Cu(1) Cl(2) Cu(3) 76.84(4) yes . . 2_566 Cu(2) Cl(2) Cu(3) 82.27(4) yes . . 2_566 Cu(2) Cl(3) Cu(3) 92.25(4) yes . . . Cu(3) Cl(4) Cu(4) 80.24(4) yes . . . Cu(5) Cl(5) Cu(8) 71.89(4) yes . . 2_656 Cu(5) Cl(6) Cu(6) 96.05(4) yes . . . Cu(6) Cl(7) Cu(6) 86.74(4) yes . . 2_656 Cu(6) Cl(7) Cu(7) 90.92(4) yes . . . Cu(6) Cl(7) Cu(7) 79.10(3) yes 2_656 . . Cu(7) Cl(8) Cu(8) 79.59(3) yes . . . Cu(9) Cl(9) Cu(12) 77.69(4) yes . . 2_557 Cu(9) Cl(10) Cu(10) 80.47(4) yes . . . Cu(10) Cl(11) Cu(11) 91.90(5) yes . . . Cu(11) Cl(12) Cu(12) 93.80(4) yes . . . Cu(1) P(1) C(1) 121.21(15) yes . . . Cu(1) P(1) C(101) 112.85(16) yes . . . Cu(1) P(1) C(107) 110.51(15) yes . . . C(1) P(1) C(101) 102.3(2) yes . . . C(1) P(1) C(107) 102.3(2) yes . . . C(101) P(1) C(107) 106.2(2) yes . . . Cu(2) P(2) C(1) 112.39(16) yes . . . Cu(2) P(2) C(2) 116.55(16) yes . . . Cu(2) P(2) C(113) 117.04(17) yes . . . C(1) P(2) C(2) 98.7(2) yes . . . C(1) P(2) C(113) 106.3(2) yes . . . C(2) P(2) C(113) 103.8(2) yes . . . Cu(3) P(3) C(2) 115.07(16) yes . . . Cu(3) P(3) C(3) 114.68(16) yes . . . Cu(3) P(3) C(119) 115.40(16) yes . . . C(2) P(3) C(3) 100.0(2) yes . . . C(2) P(3) C(119) 105.1(2) yes . . . C(3) P(3) C(119) 104.8(2) yes . . . Cu(4) P(4) C(3) 113.56(15) yes . . . Cu(4) P(4) C(125) 114.78(18) yes . . . Cu(4) P(4) C(131) 114.6(2) yes . . . C(3) P(4) C(125) 103.9(2) yes . . . C(3) P(4) C(131) 103.9(2) yes . . . C(125) P(4) C(131) 104.9(2) yes . . . Cu(5) P(5) C(4) 116.99(14) yes . . . Cu(5) P(5) C(201) 116.03(14) yes . . . Cu(5) P(5) C(207) 112.98(16) yes . . . C(4) P(5) C(201) 102.4(2) yes . . . C(4) P(5) C(207) 102.3(2) yes . . . C(201) P(5) C(207) 104.4(2) yes . . . Cu(6) P(6) C(4) 112.49(15) yes . . . Cu(6) P(6) C(5) 113.90(15) yes . . . Cu(6) P(6) C(213) 118.89(14) yes . . . C(4) P(6) C(5) 96.6(2) yes . . . C(4) P(6) C(213) 107.2(2) yes . . . C(5) P(6) C(213) 105.2(2) yes . . . Cu(7) P(7) C(5) 117.84(16) yes . . . Cu(7) P(7) C(6) 113.65(15) yes . . . Cu(7) P(7) C(219) 113.94(13) yes . . . C(5) P(7) C(6) 98.7(2) yes . . . C(5) P(7) C(219) 105.1(2) yes . . . C(6) P(7) C(219) 105.9(2) yes . . . Cu(8) P(8) C(6) 113.33(15) yes . . . Cu(8) P(8) C(225) 113.14(16) yes . . . Cu(8) P(8) C(231) 116.92(18) yes . . . C(6) P(8) C(225) 104.1(2) yes . . . C(6) P(8) C(231) 101.8(2) yes . . . C(225) P(8) C(231) 106.2(2) yes . . . Cu(9) P(9) C(7) 107.58(16) yes . . . Cu(9) P(9) C(301) 123.67(18) yes . . . Cu(9) P(9) C(307) 112.90(19) yes . . . C(7) P(9) C(301) 106.4(2) yes . . . C(7) P(9) C(307) 101.4(2) yes . . . C(301) P(9) C(307) 102.5(2) yes . . . Cu(10) P(10) C(7) 114.30(18) yes . . . Cu(10) P(10) C(8) 114.30(17) yes . . . Cu(10) P(10) C(313) 117.09(16) yes . . . C(7) P(10) C(8) 98.9(2) yes . . . C(7) P(10) C(313) 103.2(2) yes . . . C(8) P(10) C(313) 107.0(2) yes . . . Cu(11) P(11) C(8) 114.25(18) yes . . . Cu(11) P(11) C(9) 112.88(16) yes . . . Cu(11) P(11) C(319) 119.11(16) yes . . . C(8) P(11) C(9) 98.4(2) yes . . . C(8) P(11) C(319) 102.6(2) yes . . . C(9) P(11) C(319) 107.2(2) yes . . . Cu(12) P(12) C(9) 118.81(17) yes . . . Cu(12) P(12) C(325) 112.70(16) yes . . . Cu(12) P(12) C(331) 115.05(18) yes . . . C(9) P(12) C(325) 103.2(2) yes . . . C(9) P(12) C(331) 102.5(2) yes . . . C(325) P(12) C(331) 102.7(2) yes . . . P(1) C(1) P(2) 114.8(2) yes . . . P(2) C(2) P(3) 114.5(2) yes . . . P(3) C(3) P(4) 114.1(2) yes . . . P(5) C(4) P(6) 116.8(2) yes . . . P(6) C(5) P(7) 115.1(2) yes . . . P(7) C(6) P(8) 114.5(2) yes . . . P(9) C(7) P(10) 113.4(2) yes . . . P(10) C(8) P(11) 114.4(2) yes . . . P(11) C(9) P(12) 114.3(2) yes . . . P(1) C(101) C(102) 118.2(3) yes . . . P(1) C(101) C(106) 124.0(3) yes . . . C(102) C(101) C(106) 117.8(4) yes . . . C(101) C(102) C(103) 121.9(4) yes . . . C(102) C(103) C(104) 119.8(5) yes . . . C(103) C(104) C(105) 118.9(5) yes . . . C(104) C(105) C(106) 120.5(5) yes . . . C(101) C(106) C(105) 121.2(4) yes . . . P(1) C(107) C(108) 122.7(4) yes . . . P(1) C(107) C(112) 117.1(3) yes . . . C(108) C(107) C(112) 120.2(5) yes . . . C(107) C(108) C(109) 118.9(4) yes . . . C(108) C(109) C(110) 120.9(4) yes . . . C(109) C(110) C(111) 120.4(5) yes . . . C(110) C(111) C(112) 119.7(5) yes . . . C(107) C(112) C(111) 120.0(4) yes . . . P(2) C(113) C(114) 123.4(4) yes . . . P(2) C(113) C(118) 117.4(4) yes . . . C(114) C(113) C(118) 119.2(6) yes . . . C(113) C(114) C(115) 120.6(5) yes . . . C(114) C(115) C(116) 120.1(7) yes . . . C(115) C(116) C(117) 120.3(8) yes . . . C(116) C(117) C(118) 120.5(8) yes . . . C(113) C(118) C(117) 119.4(6) yes . . . P(3) C(119) C(120) 123.6(4) yes . . . P(3) C(119) C(124) 117.8(5) yes . . . C(120) C(119) C(124) 118.5(6) yes . . . C(119) C(120) C(121) 121.1(5) yes . . . C(120) C(121) C(122) 119.8(7) yes . . . C(121) C(122) C(123) 120.2(10) yes . . . C(122) C(123) C(124) 120.1(10) yes . . . C(119) C(124) C(123) 120.2(8) yes . . . P(4) C(125) C(126) 124.0(4) yes . . . P(4) C(125) C(130) 120.2(6) yes . . . C(126) C(125) C(130) 114.7(7) yes . . . C(125) C(126) C(127) 122.7(6) yes . . . C(126) C(127) C(128) 120.0(8) yes . . . C(127) C(128) C(129) 116.8(10) yes . . . C(128) C(129) C(130) 117.6(11) yes . . . C(125) C(130) C(129) 122.4(9) yes . . . P(4) C(131) C(132) 123.7(4) yes . . . P(4) C(131) C(136) 116.4(5) yes . . . C(132) C(131) C(136) 119.7(6) yes . . . C(131) C(132) C(133) 120.3(6) yes . . . C(132) C(133) C(134) 120.3(7) yes . . . C(133) C(134) C(135) 120.2(8) yes . . . C(134) C(135) C(136) 119.0(8) yes . . . C(131) C(136) C(135) 120.2(7) yes . . . P(5) C(201) C(202) 122.2(3) yes . . . P(5) C(201) C(206) 119.3(3) yes . . . C(202) C(201) C(206) 118.4(4) yes . . . C(201) C(202) C(203) 120.8(4) yes . . . C(202) C(203) C(204) 119.4(4) yes . . . C(203) C(204) C(205) 121.0(5) yes . . . C(204) C(205) C(206) 119.6(4) yes . . . C(201) C(206) C(205) 120.7(4) yes . . . P(5) C(207) C(208) 124.3(4) yes . . . P(5) C(207) C(212) 117.7(3) yes . . . C(208) C(207) C(212) 118.0(4) yes . . . C(207) C(208) C(209) 121.0(5) yes . . . C(208) C(209) C(210) 120.2(4) yes . . . C(209) C(210) C(211) 119.7(5) yes . . . C(210) C(211) C(212) 120.2(5) yes . . . C(207) C(212) C(211) 121.0(4) yes . . . P(6) C(213) C(214) 123.2(3) yes . . . P(6) C(213) C(218) 117.6(3) yes . . . C(214) C(213) C(218) 119.3(4) yes . . . C(213) C(214) C(215) 119.7(4) yes . . . C(214) C(215) C(216) 120.3(5) yes . . . C(215) C(216) C(217) 120.4(5) yes . . . C(216) C(217) C(218) 119.8(5) yes . . . C(213) C(218) C(217) 120.4(5) yes . . . P(7) C(219) C(220) 122.9(3) yes . . . P(7) C(219) C(224) 117.9(3) yes . . . C(220) C(219) C(224) 119.2(5) yes . . . C(219) C(220) C(221) 120.6(4) yes . . . C(220) C(221) C(222) 119.9(5) yes . . . C(221) C(222) C(223) 119.7(6) yes . . . C(222) C(223) C(224) 120.4(5) yes . . . C(219) C(224) C(223) 120.1(5) yes . . . P(8) C(225) C(226) 123.5(4) yes . . . P(8) C(225) C(230) 117.4(4) yes . . . C(226) C(225) C(230) 119.0(5) yes . . . C(225) C(226) C(227) 119.6(5) yes . . . C(226) C(227) C(228) 121.2(7) yes . . . C(227) C(228) C(229) 119.5(8) yes . . . C(228) C(229) C(230) 120.3(6) yes . . . C(225) C(230) C(229) 120.4(5) yes . . . P(8) C(231) C(232) 118.4(4) yes . . . P(8) C(231) C(236) 122.5(4) yes . . . C(232) C(231) C(236) 119.1(5) yes . . . C(231) C(232) C(233) 119.3(6) yes . . . C(232) C(233) C(234) 121.7(8) yes . . . C(233) C(234) C(235) 119.5(8) yes . . . C(234) C(235) C(236) 120.5(6) yes . . . C(231) C(236) C(235) 119.9(6) yes . . . P(9) C(301) C(302) 123.4(4) yes . . . P(9) C(301) C(306) 118.0(4) yes . . . C(302) C(301) C(306) 118.3(5) yes . . . C(301) C(302) C(303) 121.1(6) yes . . . C(302) C(303) C(304) 119.9(8) yes . . . C(303) C(304) C(305) 120.9(8) yes . . . C(304) C(305) C(306) 119.3(6) yes . . . C(301) C(306) C(305) 120.5(6) yes . . . P(9) C(307) C(308) 122.5(5) yes . . . P(9) C(307) C(312) 117.4(3) yes . . . C(308) C(307) C(312) 120.1(5) yes . . . C(307) C(308) C(309) 118.7(6) yes . . . C(308) C(309) C(310) 121.0(5) yes . . . C(309) C(310) C(311) 121.0(6) yes . . . C(310) C(311) C(312) 119.0(6) yes . . . C(307) C(312) C(311) 120.1(5) yes . . . P(10) C(313) C(314) 123.2(4) yes . . . P(10) C(313) C(318) 117.8(4) yes . . . C(314) C(313) C(318) 119.0(5) yes . . . C(313) C(314) C(315) 120.9(6) yes . . . C(314) C(315) C(316) 118.7(8) yes . . . C(315) C(316) C(317) 120.9(7) yes . . . C(316) C(317) C(318) 120.3(6) yes . . . C(313) C(318) C(317) 120.1(6) yes . . . P(11) C(319) C(320) 122.6(3) yes . . . P(11) C(319) C(324) 117.3(4) yes . . . C(320) C(319) C(324) 120.0(5) yes . . . C(319) C(320) C(321) 119.1(5) yes . . . C(320) C(321) C(322) 121.1(7) yes . . . C(321) C(322) C(323) 120.2(7) yes . . . C(322) C(323) C(324) 120.3(6) yes . . . C(319) C(324) C(323) 119.2(6) yes . . . P(12) C(325) C(326) 122.2(3) yes . . . P(12) C(325) C(330) 117.8(4) yes . . . C(326) C(325) C(330) 119.9(5) yes . . . C(325) C(326) C(327) 120.2(5) yes . . . C(326) C(327) C(328) 120.1(6) yes . . . C(327) C(328) C(329) 120.0(6) yes . . . C(328) C(329) C(330) 120.2(5) yes . . . C(325) C(330) C(329) 119.5(5) yes . . . P(12) C(331) C(332) 124.1(3) yes . . . P(12) C(331) C(336) 117.5(4) yes . . . C(332) C(331) C(336) 118.4(4) yes . . . C(331) C(332) C(333) 121.3(5) yes . . . C(332) C(333) C(334) 119.7(6) yes . . . C(333) C(334) C(335) 119.4(5) yes . . . C(334) C(335) C(336) 120.6(5) yes . . . C(331) C(336) C(335) 120.6(5) yes . . . Cl(21) C(401) Cl(22) 111.1(11) yes . . . Cl(23) C(402) Cl(24) 121.5(13) yes . . . P(1) C(1) H(1) 108.7 no . . . P(1) C(1) H(2) 108.3 no . . . P(2) C(1) H(1) 108.2 no . . . P(2) C(1) H(2) 107.8 no . . . H(1) C(1) H(2) 109.1 no . . . P(2) C(2) H(3) 108.5 no . . . P(2) C(2) H(4) 108.5 no . . . P(3) C(2) H(3) 108.3 no . . . P(3) C(2) H(4) 108.3 no . . . H(3) C(2) H(4) 108.5 no . . . P(3) C(3) H(5) 108.3 no . . . P(3) C(3) H(6) 108.4 no . . . P(4) C(3) H(5) 108.6 no . . . P(4) C(3) H(6) 108.7 no . . . H(5) C(3) H(6) 108.8 no . . . P(5) C(4) H(7) 107.7 no . . . P(5) C(4) H(8) 107.5 no . . . P(6) C(4) H(7) 107.8 no . . . P(6) C(4) H(8) 107.6 no . . . H(7) C(4) H(8) 109.1 no . . . P(6) C(5) H(9) 108.3 no . . . P(6) C(5) H(10) 107.9 no . . . P(7) C(5) H(9) 108.6 no . . . P(7) C(5) H(10) 108.2 no . . . H(9) C(5) H(10) 108.5 no . . . P(7) C(6) H(11) 108.9 no . . . P(7) C(6) H(12) 108.5 no . . . P(8) C(6) H(11) 108.5 no . . . P(8) C(6) H(12) 108.1 no . . . H(11) C(6) H(12) 108.1 no . . . P(9) C(7) H(13) 108.9 no . . . P(9) C(7) H(14) 108.8 no . . . P(10) C(7) H(13) 108.6 no . . . P(10) C(7) H(14) 108.4 no . . . H(13) C(7) H(14) 108.7 no . . . P(10) C(8) H(15) 108.5 no . . . P(10) C(8) H(16) 108.7 no . . . P(11) C(8) H(15) 108.1 no . . . P(11) C(8) H(16) 108.4 no . . . H(15) C(8) H(16) 108.5 no . . . P(11) C(9) H(17) 108.2 no . . . P(11) C(9) H(18) 108.4 no . . . P(12) C(9) H(17) 108.3 no . . . P(12) C(9) H(18) 108.6 no . . . H(17) C(9) H(18) 109.0 no . . . C(101) C(102) H(19) 119.1 no . . . C(103) C(102) H(19) 119.1 no . . . C(102) C(103) H(20) 119.4 no . . . C(104) C(103) H(20) 120.7 no . . . C(103) C(104) H(21) 119.9 no . . . C(105) C(104) H(21) 121.2 no . . . C(104) C(105) H(22) 120.2 no . . . C(106) C(105) H(22) 119.3 no . . . C(101) C(106) H(23) 119.3 no . . . C(105) C(106) H(23) 119.5 no . . . C(107) C(108) H(24) 120.5 no . . . C(109) C(108) H(24) 120.5 no . . . C(108) C(109) H(25) 120.3 no . . . C(110) C(109) H(25) 118.9 no . . . C(109) C(110) H(26) 119.3 no . . . C(111) C(110) H(26) 120.4 no . . . C(110) C(111) H(27) 120.1 no . . . C(112) C(111) H(27) 120.2 no . . . C(107) C(112) H(28) 119.7 no . . . C(111) C(112) H(28) 120.3 no . . . C(113) C(114) H(29) 119.6 no . . . C(115) C(114) H(29) 119.8 no . . . C(114) C(115) H(30) 119.8 no . . . C(116) C(115) H(30) 120.1 no . . . C(115) C(116) H(31) 118.4 no . . . C(117) C(116) H(31) 121.4 no . . . C(116) C(117) H(32) 119.3 no . . . C(118) C(117) H(32) 120.2 no . . . C(113) C(118) H(33) 119.2 no . . . C(117) C(118) H(33) 121.4 no . . . C(119) C(120) H(34) 119.3 no . . . C(121) C(120) H(34) 119.6 no . . . C(120) C(121) H(35) 119.7 no . . . C(122) C(121) H(35) 120.4 no . . . C(121) C(122) H(36) 119.4 no . . . C(123) C(122) H(36) 120.3 no . . . C(122) C(123) H(37) 118.6 no . . . C(124) C(123) H(37) 120.5 no . . . C(119) C(124) H(38) 120.6 no . . . C(123) C(124) H(38) 118.9 no . . . C(125) C(126) H(39) 118.5 no . . . C(127) C(126) H(39) 118.8 no . . . C(126) C(127) H(40) 120.8 no . . . C(128) C(127) H(40) 119.2 no . . . C(127) C(128) H(41) 122.3 no . . . C(129) C(128) H(41) 120.1 no . . . C(128) C(129) H(42) 118.9 no . . . C(130) C(129) H(42) 122.9 no . . . C(125) C(130) H(43) 121.2 no . . . C(129) C(130) H(43) 116.4 no . . . C(131) C(132) H(44) 119.6 no . . . C(133) C(132) H(44) 120.1 no . . . C(132) C(133) H(45) 120.2 no . . . C(134) C(133) H(45) 119.4 no . . . C(133) C(134) H(46) 119.3 no . . . C(135) C(134) H(46) 120.5 no . . . C(134) C(135) H(47) 122.1 no . . . C(136) C(135) H(47) 118.7 no . . . C(131) C(136) H(48) 119.3 no . . . C(135) C(136) H(48) 120.4 no . . . C(201) C(202) H(49) 119.3 no . . . C(203) C(202) H(49) 119.9 no . . . C(202) C(203) H(50) 120.4 no . . . C(204) C(203) H(50) 120.2 no . . . C(203) C(204) H(51) 119.7 no . . . C(205) C(204) H(51) 119.2 no . . . C(204) C(205) H(108) 120.3 no . . . C(206) C(205) H(108) 120.1 no . . . C(201) C(206) H(52) 119.6 no . . . C(205) C(206) H(52) 119.8 no . . . C(207) C(208) H(53) 119.0 no . . . C(209) C(208) H(53) 120.0 no . . . C(208) C(209) H(54) 120.1 no . . . C(210) C(209) H(54) 119.8 no . . . C(209) C(210) H(55) 120.8 no . . . C(211) C(210) H(55) 119.5 no . . . C(210) C(211) H(56) 120.0 no . . . C(212) C(211) H(56) 119.8 no . . . C(207) C(212) H(57) 119.3 no . . . C(211) C(212) H(57) 119.7 no . . . C(213) C(214) H(58) 120.1 no . . . C(215) C(214) H(58) 120.3 no . . . C(214) C(215) H(59) 119.6 no . . . C(216) C(215) H(59) 120.0 no . . . C(215) C(216) H(60) 119.7 no . . . C(217) C(216) H(60) 119.9 no . . . C(216) C(217) H(61) 119.7 no . . . C(218) C(217) H(61) 120.4 no . . . C(213) C(218) H(62) 119.3 no . . . C(217) C(218) H(62) 120.2 no . . . C(219) C(220) H(63) 119.6 no . . . C(221) C(220) H(63) 119.8 no . . . C(220) C(221) H(64) 119.9 no . . . C(222) C(221) H(64) 120.3 no . . . C(221) C(222) H(65) 120.6 no . . . C(223) C(222) H(65) 119.7 no . . . C(222) C(223) H(66) 120.0 no . . . C(224) C(223) H(66) 119.5 no . . . C(219) C(224) H(67) 119.5 no . . . C(223) C(224) H(67) 120.4 no . . . C(225) C(226) H(68) 120.5 no . . . C(227) C(226) H(68) 119.9 no . . . C(226) C(227) H(69) 120.2 no . . . C(228) C(227) H(69) 118.6 no . . . C(227) C(228) H(70) 119.3 no . . . C(229) C(228) H(70) 121.2 no . . . C(228) C(229) H(71) 120.0 no . . . C(230) C(229) H(71) 119.8 no . . . C(225) C(230) H(72) 119.4 no . . . C(229) C(230) H(72) 120.2 no . . . C(231) C(232) H(73) 120.1 no . . . C(233) C(232) H(73) 120.6 no . . . C(232) C(233) H(74) 118.6 no . . . C(234) C(233) H(74) 119.6 no . . . C(233) C(234) H(75) 120.4 no . . . C(235) C(234) H(75) 120.1 no . . . C(234) C(235) H(76) 120.0 no . . . C(236) C(235) H(76) 119.5 no . . . C(231) C(236) H(77) 120.1 no . . . C(235) C(236) H(77) 120.0 no . . . C(301) C(302) H(78) 119.5 no . . . C(303) C(302) H(78) 119.4 no . . . C(302) C(303) H(79) 119.4 no . . . C(304) C(303) H(79) 120.7 no . . . C(303) C(304) H(80) 119.1 no . . . C(305) C(304) H(80) 119.9 no . . . C(304) C(305) H(81) 121.4 no . . . C(306) C(305) H(81) 119.3 no . . . C(301) C(306) H(82) 119.4 no . . . C(305) C(306) H(82) 120.1 no . . . C(307) C(308) H(83) 120.3 no . . . C(309) C(308) H(83) 121.0 no . . . C(308) C(309) H(84) 120.1 no . . . C(310) C(309) H(84) 118.9 no . . . C(309) C(310) H(85) 120.0 no . . . C(311) C(310) H(85) 119.1 no . . . C(310) C(311) H(86) 120.4 no . . . C(312) C(311) H(86) 120.5 no . . . C(307) C(312) H(87) 120.1 no . . . C(311) C(312) H(87) 119.7 no . . . C(313) C(314) H(88) 118.7 no . . . C(315) C(314) H(88) 120.4 no . . . C(314) C(315) H(89) 120.4 no . . . C(316) C(315) H(89) 120.9 no . . . C(315) C(316) H(90) 120.0 no . . . C(317) C(316) H(90) 119.0 no . . . C(316) C(317) H(91) 120.2 no . . . C(318) C(317) H(91) 119.4 no . . . C(313) C(318) H(92) 120.1 no . . . C(317) C(318) H(92) 119.8 no . . . C(319) C(320) H(93) 120.8 no . . . C(321) C(320) H(93) 120.1 no . . . C(320) C(321) H(94) 118.8 no . . . C(322) C(321) H(94) 120.1 no . . . C(321) C(322) H(95) 120.2 no . . . C(323) C(322) H(95) 119.6 no . . . C(322) C(323) H(96) 119.8 no . . . C(324) C(323) H(96) 120.0 no . . . C(319) C(324) H(97) 120.7 no . . . C(323) C(324) H(97) 120.1 no . . . C(325) C(326) H(98) 120.0 no . . . C(327) C(326) H(98) 119.8 no . . . C(326) C(327) H(99) 119.6 no . . . C(328) C(327) H(99) 120.3 no . . . C(327) C(328) H(100) 120.4 no . . . C(329) C(328) H(100) 119.5 no . . . C(328) C(329) H(101) 120.1 no . . . C(330) C(329) H(101) 119.7 no . . . C(325) C(330) H(102) 120.2 no . . . C(329) C(330) H(102) 120.3 no . . . C(331) C(332) H(103) 119.1 no . . . C(333) C(332) H(103) 119.6 no . . . C(332) C(333) H(104) 120.1 no . . . C(334) C(333) H(104) 120.2 no . . . C(333) C(334) H(105) 120.5 no . . . C(335) C(334) H(105) 120.1 no . . . C(334) C(335) H(106) 119.7 no . . . C(336) C(335) H(106) 119.7 no . . . C(331) C(336) H(107) 119.7 no . . . C(335) C(336) H(107) 119.7 no . . . Cl(21) C(401) H(109) 109.4 no . . . Cl(21) C(401) H(110) 109.4 no . . . Cl(22) C(401) H(109) 109.4 no . . . Cl(22) C(401) H(110) 109.4 no . . . H(109) C(401) H(110) 108.0 no . . . Cl(23) C(402) H(111) 106.9 no . . . Cl(23) C(402) H(112) 107.0 no . . . Cl(24) C(402) H(111) 107.0 no . . . Cl(24) C(402) H(112) 107.0 no . . . H(111) C(402) H(112) 106.7 no . . . # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.078 0.500 1.000 859 53 ' ' 2 0.159 0.949 0.565 12 1 ' ' 3 0.246 0.897 0.324 11 1 ' ' 4 0.397 0.473 0.417 11 1 ' ' 5 0.489 0.858 0.965 27 1 ' ' 6 0.511 0.142 0.035 27 1 ' ' 7 0.603 0.527 0.583 11 1 ' ' 8 0.754 0.103 0.676 11 1 ' ' 9 0.841 0.051 0.435 12 1 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== data__compound1c-revised #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731695' # CHEMICAL DATA _chemical_formula_sum 'C78 H72 Cu8 I8 P8 ' _chemical_formula_moiety 'C78 H72 Cu8 I8 P8 ' _chemical_formula_weight 2780.82 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.395(4) _cell_length_b 14.453(5) _cell_length_c 23.562(8) _cell_angle_alpha 90.0000 _cell_angle_beta 93.1976(10) _cell_angle_gamma 90.0000 _cell_volume 4214(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6056 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.191 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632.00 _exptl_absorpt_coefficient_mu 5.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.775 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 38767 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.20 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9071 _reflns_number_gt 5037 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1388 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 9071 _refine_ls_number_parameters 462 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0649P)^2^+92.4846P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 2.73 _refine_diff_density_min -1.51 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.78043(7) 0.04293(6) 0.58859(3) 0.0355(2) Uani 1.00 1 d . . . I(2) I 0.92222(7) -0.13977(6) 0.49265(4) 0.0431(2) Uani 1.00 1 d . . . I(3) I 1.02866(8) -0.28451(6) 0.36645(4) 0.0479(2) Uani 1.00 1 d . . . I(4) I 1.34274(9) -0.26608(8) 0.32832(4) 0.0577(3) Uani 1.00 1 d . . . Cu(1) Cu 0.78468(15) 0.23162(12) 0.58116(7) 0.0482(4) Uani 1.00 1 d . . . Cu(2) Cu 0.88437(13) 0.03843(11) 0.49513(6) 0.0364(3) Uani 1.00 1 d . . . Cu(3) Cu 1.01010(12) -0.10570(10) 0.39799(7) 0.0350(3) Uani 1.00 1 d . . . Cu(4) Cu 1.16558(14) -0.17273(11) 0.31732(7) 0.0418(4) Uani 1.00 1 d . . . P(1) P 0.7338(2) 0.2794(2) 0.49394(13) 0.0293(6) Uani 1.00 1 d . . . P(2) P 0.8142(2) 0.11492(19) 0.42002(12) 0.0246(6) Uani 1.00 1 d . . . P(3) P 0.9389(2) -0.0039(2) 0.33506(13) 0.0255(6) Uani 1.00 1 d . . . P(4) P 1.1096(2) -0.0690(2) 0.25336(13) 0.0309(7) Uani 1.00 1 d . . . C(1) C 0.8077(9) 0.2411(7) 0.4321(5) 0.030(2) Uani 1.00 1 d . . . C(2) C 0.9044(8) 0.1124(7) 0.3609(5) 0.028(2) Uani 1.00 1 d . . . C(3) C 1.0385(9) 0.0303(7) 0.2842(4) 0.029(2) Uani 1.00 1 d . . . C(4) C 0.7382(9) 0.4061(7) 0.4864(4) 0.029(2) Uani 1.00 1 d . . . C(5) C 0.8240(11) 0.4499(8) 0.4637(6) 0.043(3) Uani 1.00 1 d . . . C(6) C 0.8301(13) 0.5461(9) 0.4597(6) 0.053(3) Uani 1.00 1 d . . . C(7) C 0.7455(12) 0.5981(8) 0.4797(6) 0.046(3) Uani 1.00 1 d . . . C(8) C 0.6618(11) 0.5561(9) 0.5022(7) 0.055(4) Uani 1.00 1 d . . . C(9) C 0.6576(10) 0.4598(9) 0.5065(7) 0.048(3) Uani 1.00 1 d . . . C(10) C 0.5938(9) 0.2527(7) 0.4751(5) 0.030(2) Uani 1.00 1 d . . . C(11) C 0.5438(10) 0.2671(9) 0.4222(6) 0.040(3) Uani 1.00 1 d . . . C(12) C 0.4380(11) 0.2416(9) 0.4095(6) 0.044(3) Uani 1.00 1 d . . . C(13) C 0.3801(11) 0.2014(10) 0.4505(7) 0.052(3) Uani 1.00 1 d . . . C(14) C 0.4223(11) 0.1890(9) 0.5029(7) 0.050(3) Uani 1.00 1 d . . . C(15) C 0.5291(11) 0.2134(8) 0.5169(6) 0.045(3) Uani 1.00 1 d . . . C(16) C 0.6817(8) 0.0852(8) 0.3878(4) 0.029(2) Uani 1.00 1 d . . . C(17) C 0.6471(9) 0.1155(8) 0.3333(4) 0.030(2) Uani 1.00 1 d . . . C(18) C 0.5467(9) 0.0888(9) 0.3091(5) 0.038(3) Uani 1.00 1 d . . . C(19) C 0.4815(12) 0.0300(11) 0.3399(7) 0.058(4) Uani 1.00 1 d . . . C(20) C 0.5165(11) 0.0010(10) 0.3931(7) 0.058(4) Uani 1.00 1 d . . . C(21) C 0.6160(10) 0.0283(8) 0.4171(5) 0.038(3) Uani 1.00 1 d . . . C(22) C 0.8188(10) -0.0432(8) 0.2925(5) 0.039(3) Uani 1.00 1 d . . . C(23) C 0.7896(12) -0.0061(11) 0.2395(6) 0.053(3) Uani 1.00 1 d . . . C(24) C 0.6947(14) -0.0399(13) 0.2117(6) 0.065(5) Uani 1.00 1 d . . . C(25) C 0.6394(16) -0.1054(13) 0.2330(12) 0.098(8) Uani 1.00 1 d . . . C(26) C 0.6656(14) -0.1414(12) 0.2860(11) 0.096(7) Uani 1.00 1 d . . . C(27) C 0.7575(12) -0.1101(9) 0.3148(7) 0.062(4) Uani 1.00 1 d . . . C(28) C 1.0142(9) -0.1079(8) 0.1962(5) 0.033(2) Uani 1.00 1 d . . . C(29) C 0.9938(11) -0.0563(8) 0.1482(5) 0.043(3) Uani 1.00 1 d . . . C(30) C 0.9167(12) -0.0847(11) 0.1074(5) 0.051(3) Uani 1.00 1 d . . . C(31) C 0.8578(9) -0.1644(8) 0.1155(5) 0.036(2) Uani 1.00 1 d . . . C(32) C 0.8778(11) -0.2181(9) 0.1625(6) 0.047(3) Uani 1.00 1 d . . . C(33) C 0.9573(10) -0.1894(8) 0.2028(5) 0.041(3) Uani 1.00 1 d . . . C(34) C 1.2157(11) -0.0131(9) 0.2160(5) 0.040(3) Uani 1.00 1 d . . . C(35) C 1.2181(11) 0.0813(10) 0.2044(6) 0.052(3) Uani 1.00 1 d . . . C(36) C 1.2999(14) 0.1210(11) 0.1744(7) 0.063(4) Uani 1.00 1 d . . . C(37) C 1.3833(12) 0.0663(13) 0.1585(7) 0.062(4) Uani 1.00 1 d . . . C(38) C 1.3818(12) -0.0264(13) 0.1681(7) 0.062(4) Uani 1.00 1 d . . . C(39) C 1.3012(10) -0.0680(9) 0.1987(6) 0.044(3) Uani 1.00 1 d . . . H(1) H 0.7761 0.2692 0.3983 0.037 Uiso 1.00 1 c R . . H(2) H 0.8816 0.2635 0.4367 0.037 Uiso 1.00 1 c R . . H(3) H 0.8708 0.1462 0.3300 0.036 Uiso 1.00 1 c R . . H(4) H 0.9700 0.1429 0.3731 0.036 Uiso 1.00 1 c R . . H(5) H 1.0025 0.0645 0.2542 0.033 Uiso 1.00 1 c R . . H(6) H 1.0909 0.0696 0.3034 0.033 Uiso 1.00 1 c R . . H(7) H 0.8831 0.4131 0.4507 0.052 Uiso 1.00 1 c R . . H(8) H 0.8921 0.5753 0.4440 0.064 Uiso 1.00 1 c R . . H(9) H 0.7465 0.6642 0.4773 0.056 Uiso 1.00 1 c R . . H(10) H 0.6030 0.5921 0.5157 0.066 Uiso 1.00 1 c R . . H(11) H 0.5976 0.4303 0.5235 0.058 Uiso 1.00 1 c R . . H(12) H 0.5842 0.2958 0.3933 0.045 Uiso 1.00 1 c R . . H(13) H 0.4045 0.2522 0.3724 0.055 Uiso 1.00 1 c R . . H(14) H 0.3065 0.1822 0.4411 0.063 Uiso 1.00 1 c R . . H(15) H 0.3793 0.1632 0.5315 0.059 Uiso 1.00 1 c R . . H(16) H 0.5601 0.2031 0.5548 0.052 Uiso 1.00 1 c R . . H(17) H 0.6937 0.1549 0.3128 0.036 Uiso 1.00 1 c R . . H(18) H 0.5229 0.1098 0.2718 0.046 Uiso 1.00 1 c R . . H(19) H 0.4139 0.0092 0.3230 0.065 Uiso 1.00 1 c R . . H(20) H 0.4693 -0.0372 0.4148 0.070 Uiso 1.00 1 c R . . H(21) H 0.6404 0.0069 0.4543 0.047 Uiso 1.00 1 c R . . H(22) H 0.8337 0.0429 0.2230 0.067 Uiso 1.00 1 c R . . H(23) H 0.6707 -0.0159 0.1750 0.074 Uiso 1.00 1 c R . . H(24) H 0.5772 -0.1294 0.2115 0.115 Uiso 1.00 1 c R . . H(25) H 0.6210 -0.1882 0.3020 0.114 Uiso 1.00 1 c R . . H(26) H 0.7787 -0.1346 0.3517 0.074 Uiso 1.00 1 c R . . H(27) H 1.0341 0.0000 0.1426 0.052 Uiso 1.00 1 c R . . H(28) H 0.9038 -0.0480 0.0728 0.062 Uiso 1.00 1 c R . . H(29) H 0.8029 -0.1820 0.0868 0.042 Uiso 1.00 1 c R . . H(30) H 0.8368 -0.2751 0.1684 0.055 Uiso 1.00 1 c R . . H(31) H 0.9723 -0.2267 0.2366 0.049 Uiso 1.00 1 c R . . H(32) H 1.1607 0.1207 0.2170 0.061 Uiso 1.00 1 c R . . H(33) H 1.2972 0.1858 0.1646 0.075 Uiso 1.00 1 c R . . H(34) H 1.4446 0.0939 0.1405 0.075 Uiso 1.00 1 c R . . H(35) H 1.4376 -0.0658 0.1540 0.074 Uiso 1.00 1 c R . . H(36) H 1.3039 -0.1333 0.2070 0.054 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0293(4) 0.0421(4) 0.0355(4) -0.0031(3) 0.0038(3) -0.0000(3) I(2) 0.0367(5) 0.0460(5) 0.0466(5) -0.0039(3) 0.0025(3) 0.0060(4) I(3) 0.0501(5) 0.0340(4) 0.0584(6) -0.0066(4) -0.0066(4) 0.0012(4) I(4) 0.0585(6) 0.0659(6) 0.0491(6) 0.0280(5) 0.0057(4) -0.0026(4) Cu(1) 0.0577(11) 0.0495(10) 0.0362(9) 0.0051(8) -0.0079(8) 0.0071(7) Cu(2) 0.0398(9) 0.0403(8) 0.0292(8) 0.0022(7) 0.0026(6) 0.0058(6) Cu(3) 0.0332(8) 0.0330(7) 0.0387(8) 0.0003(6) 0.0012(6) 0.0071(6) Cu(4) 0.0467(10) 0.0394(8) 0.0392(9) 0.0104(7) 0.0005(7) 0.0034(7) P(1) 0.0291(17) 0.0290(15) 0.0300(16) 0.0050(12) 0.0029(13) 0.0006(12) P(2) 0.0226(15) 0.0248(14) 0.0266(15) 0.0000(11) 0.0016(12) -0.0025(11) P(3) 0.0238(15) 0.0239(13) 0.0288(15) 0.0015(11) 0.0006(12) -0.0022(12) P(4) 0.0316(17) 0.0306(15) 0.0306(16) 0.0046(12) 0.0019(13) -0.0029(12) C(1) 0.025(6) 0.032(6) 0.034(6) 0.000(4) 0.012(5) -0.002(5) C(2) 0.022(6) 0.027(5) 0.036(6) 0.003(4) 0.001(5) 0.003(4) C(3) 0.035(6) 0.024(5) 0.028(6) 0.004(4) -0.002(5) -0.000(4) C(4) 0.028(6) 0.031(6) 0.028(6) 0.012(5) 0.003(5) -0.003(4) C(5) 0.052(8) 0.029(6) 0.051(8) 0.008(5) 0.024(6) 0.001(5) C(6) 0.083(11) 0.035(7) 0.042(8) -0.016(7) 0.018(7) -0.001(6) C(7) 0.056(9) 0.022(6) 0.059(9) 0.003(6) -0.010(7) -0.008(6) C(8) 0.038(8) 0.037(7) 0.090(12) 0.012(6) -0.001(8) -0.016(7) C(9) 0.028(7) 0.035(7) 0.082(10) -0.003(5) 0.004(7) -0.009(7) C(10) 0.034(6) 0.023(5) 0.033(6) 0.009(4) 0.006(5) 0.008(4) C(11) 0.026(7) 0.040(7) 0.056(8) 0.002(5) 0.023(6) 0.000(6) C(12) 0.042(8) 0.046(7) 0.046(8) 0.006(6) 0.004(6) 0.009(6) C(13) 0.036(8) 0.045(8) 0.074(11) 0.007(6) -0.000(7) -0.005(7) C(14) 0.038(8) 0.031(7) 0.085(11) -0.004(5) 0.027(8) 0.005(7) C(15) 0.055(9) 0.027(6) 0.053(8) 0.012(6) 0.013(6) 0.007(5) C(16) 0.019(5) 0.042(6) 0.026(6) -0.001(5) 0.002(4) -0.008(5) C(17) 0.026(6) 0.037(6) 0.028(6) 0.002(5) 0.008(5) -0.002(5) C(18) 0.025(6) 0.047(7) 0.041(7) -0.002(5) -0.009(5) -0.014(6) C(19) 0.046(8) 0.057(9) 0.068(10) -0.013(7) -0.025(7) -0.007(7) C(20) 0.035(8) 0.046(8) 0.092(12) -0.021(6) -0.006(8) 0.014(8) C(21) 0.032(7) 0.038(6) 0.044(7) -0.008(5) -0.001(5) 0.013(5) C(22) 0.037(7) 0.032(6) 0.047(7) 0.008(5) -0.007(6) -0.015(5) C(23) 0.052(9) 0.066(9) 0.041(8) 0.031(7) -0.004(6) -0.013(7) C(24) 0.062(10) 0.082(12) 0.046(9) 0.026(9) -0.035(8) -0.029(8) C(25) 0.070(13) 0.044(10) 0.17(2) 0.009(9) -0.056(14) -0.040(12) C(26) 0.047(10) 0.049(10) 0.19(2) 0.004(8) -0.054(13) -0.009(12) C(27) 0.043(8) 0.035(7) 0.103(13) -0.006(6) -0.030(8) -0.003(7) C(28) 0.030(6) 0.040(6) 0.029(6) 0.009(5) 0.005(5) -0.006(5) C(29) 0.046(8) 0.037(7) 0.046(8) 0.000(5) -0.004(6) -0.003(5) C(30) 0.048(8) 0.069(10) 0.036(7) 0.006(7) 0.005(6) 0.004(7) C(31) 0.022(6) 0.041(7) 0.043(7) 0.001(5) -0.006(5) -0.011(5) C(32) 0.043(8) 0.042(7) 0.056(9) -0.000(6) -0.009(6) -0.010(6) C(33) 0.040(7) 0.034(6) 0.048(8) 0.005(5) -0.000(6) -0.003(5) C(34) 0.049(8) 0.044(7) 0.028(6) -0.004(6) -0.006(5) -0.001(5) C(35) 0.045(9) 0.052(8) 0.062(9) 0.009(7) 0.021(7) 0.013(7) C(36) 0.066(11) 0.052(9) 0.073(11) -0.003(8) 0.014(9) 0.010(8) C(37) 0.040(9) 0.088(13) 0.057(10) -0.017(8) -0.005(7) 0.007(9) C(38) 0.036(8) 0.091(13) 0.060(10) 0.001(8) 0.012(7) -0.011(9) C(39) 0.036(8) 0.048(8) 0.050(8) 0.015(6) 0.011(6) 0.001(6) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Cu(1) 2.7334(19) yes . . I(1) Cu(2) 2.6134(16) yes . . I(1) Cu(3) 2.7519(17) yes . 3_756 I(2) Cu(2) 2.6191(18) yes . . I(2) Cu(2) 2.8104(18) yes . 3_756 I(2) Cu(3) 2.5835(18) yes . . I(3) Cu(1) 2.673(2) yes . 3_756 I(3) Cu(3) 2.7023(17) yes . . I(3) Cu(4) 2.6551(19) yes . . I(4) Cu(1) 2.769(2) yes . 3_756 I(4) Cu(4) 2.578(2) yes . . Cu(1) Cu(4) 2.581(2) yes . 3_756 Cu(1) P(1) 2.226(3) yes . . Cu(2) P(2) 2.222(3) yes . . Cu(3) P(3) 2.236(3) yes . . Cu(4) P(4) 2.210(3) yes . . P(1) C(1) 1.849(12) yes . . P(1) C(4) 1.841(11) yes . . P(1) C(10) 1.808(12) yes . . P(2) C(1) 1.848(11) yes . . P(2) C(2) 1.835(12) yes . . P(2) C(16) 1.822(11) yes . . P(3) C(2) 1.846(11) yes . . P(3) C(3) 1.836(12) yes . . P(3) C(22) 1.837(12) yes . . P(4) C(3) 1.853(11) yes . . P(4) C(28) 1.832(11) yes . . P(4) C(34) 1.811(13) yes . . C(4) C(5) 1.372(18) yes . . C(4) C(9) 1.370(18) yes . . C(5) C(6) 1.396(18) yes . . C(6) C(7) 1.39(2) yes . . C(7) C(8) 1.34(2) yes . . C(8) C(9) 1.396(19) yes . . C(10) C(11) 1.376(17) yes . . C(10) C(15) 1.422(18) yes . . C(11) C(12) 1.380(18) yes . . C(12) C(13) 1.36(2) yes . . C(13) C(14) 1.33(2) yes . . C(14) C(15) 1.39(2) yes . . C(16) C(17) 1.400(15) yes . . C(16) C(21) 1.370(17) yes . . C(17) C(18) 1.395(16) yes . . C(18) C(19) 1.40(2) yes . . C(19) C(20) 1.37(2) yes . . C(20) C(21) 1.385(18) yes . . C(22) C(23) 1.390(19) yes . . C(22) C(27) 1.35(2) yes . . C(23) C(24) 1.40(2) yes . . C(24) C(25) 1.29(2) yes . . C(25) C(26) 1.37(3) yes . . C(26) C(27) 1.37(2) yes . . C(28) C(29) 1.365(17) yes . . C(28) C(33) 1.386(17) yes . . C(29) C(30) 1.380(19) yes . . C(30) C(31) 1.38(2) yes . . C(31) C(32) 1.365(19) yes . . C(32) C(33) 1.394(19) yes . . C(34) C(35) 1.39(2) yes . . C(34) C(39) 1.403(19) yes . . C(35) C(36) 1.39(2) yes . . C(36) C(37) 1.37(2) yes . . C(37) C(38) 1.36(2) yes . . C(38) C(39) 1.40(2) yes . . C(1) H(1) 0.959 no . . C(1) H(2) 0.972 no . . C(2) H(3) 0.952 no . . C(2) H(4) 0.955 no . . C(3) H(5) 0.951 no . . C(3) H(6) 0.958 no . . C(5) H(7) 0.969 no . . C(6) H(8) 0.968 no . . C(7) H(9) 0.957 no . . C(8) H(10) 0.963 no . . C(9) H(11) 0.965 no . . C(11) H(12) 0.962 no . . C(12) H(13) 0.959 no . . C(13) H(14) 0.968 no . . C(14) H(15) 0.958 no . . C(15) H(16) 0.964 no . . C(17) H(17) 0.961 no . . C(18) H(18) 0.960 no . . C(19) H(19) 0.956 no . . C(20) H(20) 0.970 no . . C(21) H(21) 0.961 no . . C(23) H(22) 0.987 no . . C(24) H(23) 0.964 no . . C(25) H(24) 0.963 no . . C(26) H(25) 0.963 no . . C(27) H(26) 0.961 no . . C(29) H(27) 0.968 no . . C(30) H(28) 0.978 no . . C(31) H(29) 0.966 no . . C(32) H(30) 0.981 no . . C(33) H(31) 0.971 no . . C(35) H(32) 0.970 no . . C(36) H(33) 0.964 no . . C(37) H(34) 0.975 no . . C(38) H(35) 0.969 no . . C(39) H(36) 0.963 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) I(1) Cu(2) 87.63(5) yes . . . Cu(1) I(1) Cu(3) 69.94(5) yes . . 3_756 Cu(2) I(1) Cu(3) 66.34(5) yes . . 3_756 Cu(2) I(2) Cu(2) 68.78(5) yes . . 3_756 Cu(2) I(2) Cu(3) 85.21(5) yes . . . Cu(2) I(2) Cu(3) 65.84(4) yes 3_756 . . Cu(1) I(3) Cu(3) 71.59(5) yes 3_756 . . Cu(1) I(3) Cu(4) 57.95(5) yes 3_756 . . Cu(3) I(3) Cu(4) 66.69(5) yes . . . Cu(1) I(4) Cu(4) 57.59(5) yes 3_756 . . I(1) Cu(1) I(3) 105.97(6) yes . . 3_756 I(1) Cu(1) I(4) 96.68(6) yes . . 3_756 I(1) Cu(1) Cu(4) 67.43(5) yes . . 3_756 I(1) Cu(1) P(1) 111.29(10) yes . . . I(3) Cu(1) I(4) 96.26(5) yes 3_756 . 3_756 I(3) Cu(1) Cu(4) 60.68(5) yes 3_756 . 3_756 I(3) Cu(1) P(1) 122.10(11) yes 3_756 . . I(4) Cu(1) Cu(4) 57.49(5) yes 3_756 . 3_756 I(4) Cu(1) P(1) 120.73(11) yes 3_756 . . Cu(4) Cu(1) P(1) 177.19(12) yes 3_756 . . I(1) Cu(2) I(2) 98.08(5) yes . . . I(1) Cu(2) I(2) 111.01(5) yes . . 3_756 I(1) Cu(2) P(2) 117.98(10) yes . . . I(2) Cu(2) I(2) 111.22(6) yes . . 3_756 I(2) Cu(2) P(2) 122.28(9) yes . . . I(2) Cu(2) P(2) 96.67(9) yes 3_756 . . I(1) Cu(3) I(2) 113.84(6) yes 3_756 . . I(1) Cu(3) I(3) 104.63(5) yes 3_756 . . I(1) Cu(3) P(3) 101.20(9) yes 3_756 . . I(2) Cu(3) I(3) 95.83(5) yes . . . I(2) Cu(3) P(3) 121.88(10) yes . . . I(3) Cu(3) P(3) 118.93(10) yes . . . I(3) Cu(4) I(4) 101.50(6) yes . . . I(3) Cu(4) Cu(1) 61.36(5) yes . . 3_756 I(3) Cu(4) P(4) 121.76(11) yes . . . I(4) Cu(4) Cu(1) 64.92(6) yes . . 3_756 I(4) Cu(4) P(4) 131.05(11) yes . . . Cu(1) Cu(4) P(4) 154.88(11) yes 3_756 . . Cu(1) P(1) C(1) 120.5(3) yes . . . Cu(1) P(1) C(4) 112.9(3) yes . . . Cu(1) P(1) C(10) 112.3(4) yes . . . C(1) P(1) C(4) 101.7(5) yes . . . C(1) P(1) C(10) 104.7(5) yes . . . C(4) P(1) C(10) 102.8(5) yes . . . Cu(2) P(2) C(1) 112.7(3) yes . . . Cu(2) P(2) C(2) 111.5(3) yes . . . Cu(2) P(2) C(16) 121.2(3) yes . . . C(1) P(2) C(2) 99.8(5) yes . . . C(1) P(2) C(16) 104.5(5) yes . . . C(2) P(2) C(16) 104.6(5) yes . . . Cu(3) P(3) C(2) 118.1(3) yes . . . Cu(3) P(3) C(3) 110.8(3) yes . . . Cu(3) P(3) C(22) 115.8(4) yes . . . C(2) P(3) C(3) 98.5(5) yes . . . C(2) P(3) C(22) 105.5(5) yes . . . C(3) P(3) C(22) 106.3(5) yes . . . Cu(4) P(4) C(3) 113.3(3) yes . . . Cu(4) P(4) C(28) 117.3(4) yes . . . Cu(4) P(4) C(34) 115.2(4) yes . . . C(3) P(4) C(28) 102.9(5) yes . . . C(3) P(4) C(34) 102.6(5) yes . . . C(28) P(4) C(34) 103.7(5) yes . . . P(1) C(1) P(2) 116.4(6) yes . . . P(2) C(2) P(3) 115.5(6) yes . . . P(3) C(3) P(4) 113.6(5) yes . . . P(1) C(4) C(5) 121.7(9) yes . . . P(1) C(4) C(9) 120.3(9) yes . . . C(5) C(4) C(9) 117.9(11) yes . . . C(4) C(5) C(6) 122.2(13) yes . . . C(5) C(6) C(7) 118.0(14) yes . . . C(6) C(7) C(8) 120.3(12) yes . . . C(7) C(8) C(9) 120.9(13) yes . . . C(4) C(9) C(8) 120.6(13) yes . . . P(1) C(10) C(11) 124.6(9) yes . . . P(1) C(10) C(15) 119.1(9) yes . . . C(11) C(10) C(15) 116.3(11) yes . . . C(10) C(11) C(12) 122.1(12) yes . . . C(11) C(12) C(13) 119.4(13) yes . . . C(12) C(13) C(14) 121.4(13) yes . . . C(13) C(14) C(15) 120.4(14) yes . . . C(10) C(15) C(14) 120.3(13) yes . . . P(2) C(16) C(17) 122.1(8) yes . . . P(2) C(16) C(21) 118.5(8) yes . . . C(17) C(16) C(21) 119.3(10) yes . . . C(16) C(17) C(18) 120.6(11) yes . . . C(17) C(18) C(19) 118.8(12) yes . . . C(18) C(19) C(20) 119.8(13) yes . . . C(19) C(20) C(21) 121.0(14) yes . . . C(16) C(21) C(20) 120.3(12) yes . . . P(3) C(22) C(23) 122.2(10) yes . . . P(3) C(22) C(27) 117.7(10) yes . . . C(23) C(22) C(27) 120.0(13) yes . . . C(22) C(23) C(24) 117.1(14) yes . . . C(23) C(24) C(25) 121.8(17) yes . . . C(24) C(25) C(26) 121.9(19) yes . . . C(25) C(26) C(27) 118.2(18) yes . . . C(22) C(27) C(26) 120.9(17) yes . . . P(4) C(28) C(29) 121.5(9) yes . . . P(4) C(28) C(33) 119.3(9) yes . . . C(29) C(28) C(33) 119.1(11) yes . . . C(28) C(29) C(30) 120.2(12) yes . . . C(29) C(30) C(31) 120.2(12) yes . . . C(30) C(31) C(32) 120.8(11) yes . . . C(31) C(32) C(33) 118.3(12) yes . . . C(28) C(33) C(32) 121.4(12) yes . . . P(4) C(34) C(35) 123.9(10) yes . . . P(4) C(34) C(39) 118.0(10) yes . . . C(35) C(34) C(39) 118.2(12) yes . . . C(34) C(35) C(36) 121.9(14) yes . . . C(35) C(36) C(37) 119.0(15) yes . . . C(36) C(37) C(38) 120.3(15) yes . . . C(37) C(38) C(39) 121.8(15) yes . . . C(34) C(39) C(38) 118.6(13) yes . . . P(1) C(1) H(1) 109.3 no . . . P(1) C(1) H(2) 108.6 no . . . P(2) C(1) H(1) 108.0 no . . . P(2) C(1) H(2) 107.3 no . . . H(1) C(1) H(2) 106.9 no . . . P(2) C(2) H(3) 108.1 no . . . P(2) C(2) H(4) 107.9 no . . . P(3) C(2) H(3) 108.2 no . . . P(3) C(2) H(4) 108.1 no . . . H(3) C(2) H(4) 108.9 no . . . P(3) C(3) H(5) 108.7 no . . . P(3) C(3) H(6) 108.3 no . . . P(4) C(3) H(5) 109.0 no . . . P(4) C(3) H(6) 108.6 no . . . H(5) C(3) H(6) 108.6 no . . . C(4) C(5) H(7) 119.1 no . . . C(6) C(5) H(7) 118.7 no . . . C(5) C(6) H(8) 120.5 no . . . C(7) C(6) H(8) 121.5 no . . . C(6) C(7) H(9) 120.4 no . . . C(8) C(7) H(9) 119.3 no . . . C(7) C(8) H(10) 120.1 no . . . C(9) C(8) H(10) 119.0 no . . . C(4) C(9) H(11) 119.2 no . . . C(8) C(9) H(11) 120.2 no . . . C(10) C(11) H(12) 118.8 no . . . C(12) C(11) H(12) 119.1 no . . . C(11) C(12) H(13) 120.9 no . . . C(13) C(12) H(13) 119.7 no . . . C(12) C(13) H(14) 119.2 no . . . C(14) C(13) H(14) 119.4 no . . . C(13) C(14) H(15) 120.1 no . . . C(15) C(14) H(15) 119.5 no . . . C(10) C(15) H(16) 119.4 no . . . C(14) C(15) H(16) 120.3 no . . . C(16) C(17) H(17) 119.0 no . . . C(18) C(17) H(17) 120.4 no . . . C(17) C(18) H(18) 120.6 no . . . C(19) C(18) H(18) 120.6 no . . . C(18) C(19) H(19) 119.5 no . . . C(20) C(19) H(19) 120.6 no . . . C(19) C(20) H(20) 119.0 no . . . C(21) C(20) H(20) 119.9 no . . . C(16) C(21) H(21) 119.2 no . . . C(20) C(21) H(21) 120.4 no . . . C(22) C(23) H(22) 120.5 no . . . C(24) C(23) H(22) 122.4 no . . . C(23) C(24) H(23) 120.2 no . . . C(25) C(24) H(23) 118.0 no . . . C(24) C(25) H(24) 119.3 no . . . C(26) C(25) H(24) 118.9 no . . . C(25) C(26) H(25) 120.7 no . . . C(27) C(26) H(25) 121.1 no . . . C(22) C(27) H(26) 118.9 no . . . C(26) C(27) H(26) 120.2 no . . . C(28) C(29) H(27) 120.0 no . . . C(30) C(29) H(27) 119.8 no . . . C(29) C(30) H(28) 119.6 no . . . C(31) C(30) H(28) 120.2 no . . . C(30) C(31) H(29) 118.7 no . . . C(32) C(31) H(29) 120.5 no . . . C(31) C(32) H(30) 121.3 no . . . C(33) C(32) H(30) 120.4 no . . . C(28) C(33) H(31) 119.3 no . . . C(32) C(33) H(31) 119.3 no . . . C(34) C(35) H(32) 119.3 no . . . C(36) C(35) H(32) 118.8 no . . . C(35) C(36) H(33) 120.4 no . . . C(37) C(36) H(33) 120.7 no . . . C(36) C(37) H(34) 120.1 no . . . C(38) C(37) H(34) 119.6 no . . . C(37) C(38) H(35) 120.3 no . . . C(39) C(38) H(35) 117.9 no . . . C(34) C(39) H(36) 120.9 no . . . C(38) C(39) H(36) 120.4 no . . . #============================================================================== #============================================================================== data__compound2-revised #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731696' # CHEMICAL DATA _chemical_formula_sum 'C80 H72 Cl6 Cu8 F6 O6 P8 S2 ' _chemical_formula_moiety 'C80 H72 Cl6 Cu8 F6 O6 P8 S2 ' _chemical_formula_weight 2276.43 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 12.222(4) _cell_length_b 14.096(5) _cell_length_c 24.830(9) _cell_angle_alpha 90.0000 _cell_angle_beta 95.3499(11) _cell_angle_gamma 90.0000 _cell_volume 4259(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5864 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280.00 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.953 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 39182 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_theta_max 27.13 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9020 _reflns_number_gt 4305 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.1814 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 9020 _refine_ls_number_parameters 345 _refine_ls_goodness_of_fit_ref 1.383 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 2.50 _refine_diff_density_min -2.02 _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu -0.17172(15) 0.22337(12) 0.04325(7) 0.0612(6) Uani 1.00 1 d . . . Cu(2) Cu -0.13669(11) 0.03515(11) -0.01709(6) 0.0348(4) Uani 1.00 1 d . . . Cu(3) Cu -0.01346(11) -0.10764(11) -0.08603(6) 0.0386(4) Uani 1.00 1 d . . . Cu(4) Cu 0.12006(12) -0.21595(11) -0.16285(6) 0.0416(4) Uani 1.00 1 d . . . Cl(1) Cl -0.1828(2) 0.0667(2) 0.07458(11) 0.0339(8) Uani 1.00 1 d . . . Cl(2) Cl -0.0600(2) -0.1157(2) 0.00204(11) 0.0305(7) Uani 1.00 1 d . . . Cl(3) Cl 0.0255(2) -0.2841(2) -0.09690(12) 0.0377(8) Uani 1.00 1 d . . . S(1) S 0.2935(3) -0.3631(2) -0.17321(15) 0.0571(12) Uani 1.00 1 d . . . P(1) P -0.2678(2) 0.2791(2) -0.02738(11) 0.0269(8) Uani 1.00 1 d . . . P(2) P -0.2178(2) 0.0992(2) -0.09085(11) 0.0214(7) Uani 1.00 1 d . . . P(3) P -0.1017(2) -0.0455(2) -0.15763(11) 0.0224(7) Uani 1.00 1 d . . . P(4) P 0.0587(2) -0.1348(2) -0.23327(12) 0.0246(8) Uani 1.00 1 d . . . F(1) F 0.2258(9) -0.4633(7) -0.0956(4) 0.120(4) Uani 1.00 1 d . . . F(2) F 0.3986(9) -0.4249(8) -0.0869(4) 0.124(4) Uani 1.00 1 d . . . F(3) F 0.3406(10) -0.5331(7) -0.1409(3) 0.127(4) Uani 1.00 1 d . . . O(1) O 0.2842(6) -0.2657(6) -0.1392(3) 0.049(2) Uiso 1.00 1 d . . . O(2) O 0.1976(8) -0.4007(7) -0.2055(4) 0.083(3) Uiso 1.00 1 d . . . O(3) O 0.3946(10) -0.3650(8) -0.1982(5) 0.105(4) Uiso 1.00 1 d . . . C(1) C -0.0226(8) -0.0300(7) -0.2170(4) 0.026(2) Uiso 1.00 1 d . . . C(2) C -0.1426(8) 0.0766(7) -0.1502(3) 0.023(2) Uiso 1.00 1 d . . . C(3) C -0.2207(8) 0.2300(7) -0.0894(4) 0.024(2) Uiso 1.00 1 d . . . C(4) C 0.3160(14) -0.4509(13) -0.1226(7) 0.078(4) Uiso 1.00 1 d . . . C(5) C 0.1613(8) -0.0806(7) -0.2706(4) 0.023(2) Uiso 1.00 1 d . . . C(6) C 0.2685(9) -0.1175(8) -0.2672(4) 0.042(3) Uiso 1.00 1 d . . . C(7) C 0.3497(10) -0.0717(9) -0.2933(4) 0.044(3) Uiso 1.00 1 d . . . C(8) C 0.3260(11) 0.0055(9) -0.3223(5) 0.056(3) Uiso 1.00 1 d . . . C(9) C 0.2217(9) 0.0442(9) -0.3300(5) 0.045(3) Uiso 1.00 1 d . . . C(10) C 0.1425(9) 0.0004(8) -0.3026(4) 0.038(3) Uiso 1.00 1 d . . . C(11) C -0.0279(8) -0.2023(7) -0.2838(4) 0.028(2) Uiso 1.00 1 d . . . C(12) C -0.0313(8) -0.1856(8) -0.3367(4) 0.035(2) Uiso 1.00 1 d . . . C(13) C -0.0948(9) -0.2447(8) -0.3753(5) 0.039(3) Uiso 1.00 1 d . . . C(14) C -0.1561(9) -0.3168(9) -0.3543(4) 0.042(3) Uiso 1.00 1 d . . . C(15) C -0.1583(9) -0.3310(9) -0.3015(5) 0.045(3) Uiso 1.00 1 d . . . C(16) C -0.0909(8) -0.2746(8) -0.2656(4) 0.035(2) Uiso 1.00 1 d . . . C(17) C -0.2240(7) -0.1117(7) -0.1807(3) 0.021(2) Uiso 1.00 1 d . . . C(18) C -0.2714(9) -0.1053(8) -0.2349(4) 0.040(3) Uiso 1.00 1 d . . . C(19) C -0.3648(9) -0.1646(8) -0.2499(4) 0.039(3) Uiso 1.00 1 d . . . C(20) C -0.4090(9) -0.2193(8) -0.2136(4) 0.041(3) Uiso 1.00 1 d . . . C(21) C -0.3618(9) -0.2238(9) -0.1615(5) 0.045(3) Uiso 1.00 1 d . . . C(22) C -0.2690(9) -0.1703(8) -0.1447(4) 0.039(3) Uiso 1.00 1 d . . . C(23) C -0.3603(7) 0.0665(7) -0.1136(3) 0.018(2) Uiso 1.00 1 d . . . C(24) C -0.4054(8) 0.0855(8) -0.1645(4) 0.032(2) Uiso 1.00 1 d . . . C(25) C -0.5146(9) 0.0603(8) -0.1797(5) 0.042(3) Uiso 1.00 1 d . . . C(26) C -0.5755(9) 0.0188(8) -0.1429(4) 0.035(2) Uiso 1.00 1 d . . . C(27) C -0.5314(8) 0.0010(7) -0.0910(4) 0.028(2) Uiso 1.00 1 d . . . C(28) C -0.4250(8) 0.0246(7) -0.0769(4) 0.028(2) Uiso 1.00 1 d . . . C(29) C -0.4135(8) 0.2565(7) -0.0311(4) 0.028(2) Uiso 1.00 1 d . . . C(30) C -0.4840(8) 0.2738(8) -0.0779(4) 0.034(2) Uiso 1.00 1 d . . . C(31) C -0.5941(8) 0.2510(7) -0.0784(4) 0.034(2) Uiso 1.00 1 d . . . C(32) C -0.6365(9) 0.2154(8) -0.0334(4) 0.039(3) Uiso 1.00 1 d . . . C(33) C -0.5677(9) 0.2014(9) 0.0117(5) 0.047(3) Uiso 1.00 1 d . . . C(34) C -0.4562(8) 0.2210(7) 0.0135(4) 0.030(2) Uiso 1.00 1 d . . . C(35) C -0.2528(8) 0.4057(7) -0.0353(4) 0.026(2) Uiso 1.00 1 d . . . C(36) C -0.1483(9) 0.4409(9) -0.0369(4) 0.042(3) Uiso 1.00 1 d . . . C(37) C -0.1293(10) 0.5375(9) -0.0362(4) 0.044(3) Uiso 1.00 1 d . . . C(38) C -0.2180(10) 0.5990(10) -0.0349(5) 0.053(3) Uiso 1.00 1 d . . . C(39) C -0.3221(9) 0.5660(8) -0.0342(4) 0.039(3) Uiso 1.00 1 d . . . C(40) C -0.3375(9) 0.4714(8) -0.0348(4) 0.039(3) Uiso 1.00 1 d . . . H(1) H 0.0262 0.0220 -0.2102 0.031 Uiso 1.00 1 c R . . H(2) H -0.0730 -0.0162 -0.2475 0.031 Uiso 1.00 1 c R . . H(3) H -0.0786 0.1153 -0.1475 0.027 Uiso 1.00 1 c R . . H(4) H -0.1889 0.0939 -0.1815 0.027 Uiso 1.00 1 c R . . H(5) H -0.1491 0.2532 -0.0937 0.029 Uiso 1.00 1 c R . . H(6) H -0.2701 0.2508 -0.1188 0.029 Uiso 1.00 1 c R . . H(7) H 0.2845 -0.1727 -0.2460 0.050 Uiso 1.00 1 c R . . H(8) H 0.4223 -0.0964 -0.2896 0.053 Uiso 1.00 1 c R . . H(9) H 0.3844 0.0346 -0.3389 0.067 Uiso 1.00 1 c R . . H(10) H 0.2066 0.0979 -0.3526 0.054 Uiso 1.00 1 c R . . H(11) H 0.0700 0.0254 -0.3058 0.046 Uiso 1.00 1 c R . . H(12) H 0.0104 -0.1346 -0.3493 0.042 Uiso 1.00 1 c R . . H(13) H -0.0940 -0.2354 -0.4132 0.047 Uiso 1.00 1 c R . . H(14) H -0.1997 -0.3555 -0.3792 0.051 Uiso 1.00 1 c R . . H(15) H -0.2026 -0.3799 -0.2886 0.054 Uiso 1.00 1 c R . . H(16) H -0.0882 -0.2851 -0.2277 0.042 Uiso 1.00 1 c R . . H(17) H -0.2410 -0.0651 -0.2604 0.048 Uiso 1.00 1 c R . . H(18) H -0.3964 -0.1650 -0.2863 0.046 Uiso 1.00 1 c R . . H(19) H -0.4740 -0.2546 -0.2235 0.050 Uiso 1.00 1 c R . . H(20) H -0.3935 -0.2648 -0.1369 0.054 Uiso 1.00 1 c R . . H(21) H -0.2382 -0.1746 -0.1082 0.047 Uiso 1.00 1 c R . . H(22) H -0.3624 0.1153 -0.1896 0.038 Uiso 1.00 1 c R . . H(23) H -0.5473 0.0715 -0.2154 0.050 Uiso 1.00 1 c R . . H(24) H -0.6493 0.0003 -0.1531 0.042 Uiso 1.00 1 c R . . H(25) H -0.5751 -0.0270 -0.0656 0.034 Uiso 1.00 1 c R . . H(26) H -0.3932 0.0114 -0.0413 0.033 Uiso 1.00 1 c R . . H(27) H -0.4548 0.2999 -0.1088 0.041 Uiso 1.00 1 c R . . H(28) H -0.6427 0.2615 -0.1100 0.041 Uiso 1.00 1 c R . . H(29) H -0.7118 0.1985 -0.0337 0.046 Uiso 1.00 1 c R . . H(30) H -0.5991 0.1795 0.0430 0.056 Uiso 1.00 1 c R . . H(31) H -0.4106 0.2097 0.0460 0.035 Uiso 1.00 1 c R . . H(32) H -0.0880 0.3983 -0.0363 0.050 Uiso 1.00 1 c R . . H(33) H -0.0571 0.5613 -0.0386 0.053 Uiso 1.00 1 c R . . H(34) H -0.2056 0.6655 -0.0350 0.064 Uiso 1.00 1 c R . . H(35) H -0.3822 0.6079 -0.0314 0.047 Uiso 1.00 1 c R . . H(36) H -0.4104 0.4477 -0.0359 0.047 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0865(13) 0.0429(11) 0.0471(11) 0.0228(9) -0.0308(9) -0.0041(8) Cu(2) 0.0306(8) 0.0403(9) 0.0316(8) 0.0075(7) -0.0068(6) 0.0020(7) Cu(3) 0.0351(8) 0.0503(10) 0.0293(8) 0.0129(7) -0.0029(6) -0.0005(7) Cu(4) 0.0465(9) 0.0401(10) 0.0379(9) 0.0063(7) 0.0025(7) 0.0032(7) Cl(1) 0.0230(14) 0.0454(19) 0.0336(16) -0.0071(13) 0.0040(12) 0.0072(14) Cl(2) 0.0254(14) 0.0354(17) 0.0302(15) -0.0040(13) 0.0008(12) 0.0080(13) Cl(3) 0.0369(16) 0.0317(18) 0.0445(18) -0.0017(14) 0.0034(14) 0.0044(15) S(1) 0.057(2) 0.057(2) 0.057(2) -0.0002(19) 0.0041(19) -0.0017(19) P(1) 0.0285(16) 0.0267(17) 0.0244(16) 0.0075(13) -0.0034(13) -0.0036(13) P(2) 0.0141(13) 0.0285(17) 0.0216(15) 0.0014(12) 0.0019(11) -0.0042(13) P(3) 0.0170(14) 0.0234(16) 0.0266(16) 0.0001(12) 0.0006(12) -0.0053(13) P(4) 0.0254(15) 0.0232(17) 0.0260(16) 0.0026(13) 0.0069(12) -0.0033(13) F(1) 0.151(9) 0.110(9) 0.111(8) 0.029(7) 0.080(7) 0.041(7) F(2) 0.137(9) 0.125(9) 0.099(8) 0.044(7) -0.052(7) -0.024(7) F(3) 0.219(12) 0.083(7) 0.073(6) 0.077(8) -0.026(7) -0.010(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) Cl(1) 2.350(3) yes . . Cu(1) Cl(3) 2.293(3) yes . 3_555 Cu(1) P(1) 2.165(3) yes . . Cu(2) Cl(1) 2.436(3) yes . . Cu(2) Cl(2) 2.355(3) yes . . Cu(2) Cl(2) 2.653(2) yes . 3_555 Cu(2) P(2) 2.194(3) yes . . Cu(3) Cl(1) 2.458(2) yes . 3_555 Cu(3) Cl(2) 2.313(3) yes . . Cu(3) Cl(3) 2.551(3) yes . . Cu(3) P(3) 2.176(2) yes . . Cu(4) Cl(3) 2.301(3) yes . . Cu(4) P(4) 2.164(3) yes . . Cu(4) O(1) 2.154(8) yes . . S(1) O(1) 1.621(9) yes . . S(1) O(2) 1.457(10) yes . . S(1) O(3) 1.434(13) yes . . S(1) C(4) 1.768(19) yes . . P(1) C(3) 1.829(10) yes . . P(1) C(29) 1.803(10) yes . . P(1) C(35) 1.807(11) yes . . P(2) C(2) 1.836(10) yes . . P(2) C(3) 1.844(10) yes . . P(2) C(23) 1.839(9) yes . . P(3) C(1) 1.850(11) yes . . P(3) C(2) 1.806(10) yes . . P(3) C(17) 1.810(9) yes . . P(4) C(1) 1.846(10) yes . . P(4) C(5) 1.798(10) yes . . P(4) C(11) 1.831(10) yes . . F(1) C(4) 1.35(2) yes . . F(2) C(4) 1.33(2) yes . . F(3) C(4) 1.29(2) yes . . C(5) C(6) 1.404(15) yes . . C(5) C(10) 1.397(15) yes . . C(6) C(7) 1.393(17) yes . . C(7) C(8) 1.322(18) yes . . C(8) C(9) 1.383(18) yes . . C(9) C(10) 1.381(17) yes . . C(11) C(12) 1.332(15) yes . . C(11) C(16) 1.378(15) yes . . C(12) C(13) 1.441(15) yes . . C(13) C(14) 1.392(17) yes . . C(14) C(15) 1.331(17) yes . . C(15) C(16) 1.402(16) yes . . C(17) C(18) 1.418(14) yes . . C(17) C(22) 1.370(15) yes . . C(18) C(19) 1.436(16) yes . . C(19) C(20) 1.337(17) yes . . C(20) C(21) 1.368(16) yes . . C(21) C(22) 1.393(16) yes . . C(23) C(24) 1.359(13) yes . . C(23) C(28) 1.391(14) yes . . C(24) C(25) 1.399(15) yes . . C(25) C(26) 1.362(17) yes . . C(26) C(27) 1.373(15) yes . . C(27) C(28) 1.357(14) yes . . C(29) C(30) 1.402(14) yes . . C(29) C(34) 1.362(15) yes . . C(30) C(31) 1.382(15) yes . . C(31) C(32) 1.370(16) yes . . C(32) C(33) 1.350(16) yes . . C(33) C(34) 1.388(16) yes . . C(35) C(36) 1.374(15) yes . . C(35) C(40) 1.390(15) yes . . C(36) C(37) 1.382(18) yes . . C(37) C(38) 1.392(18) yes . . C(38) C(39) 1.356(17) yes . . C(39) C(40) 1.346(17) yes . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(2) H(3) 0.950 no . . C(2) H(4) 0.950 no . . C(3) H(5) 0.950 no . . C(3) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(8) H(9) 0.950 no . . C(9) H(10) 0.950 no . . C(10) H(11) 0.950 no . . C(12) H(12) 0.950 no . . C(13) H(13) 0.950 no . . C(14) H(14) 0.950 no . . C(15) H(15) 0.950 no . . C(16) H(16) 0.950 no . . C(18) H(17) 0.950 no . . C(19) H(18) 0.950 no . . C(20) H(19) 0.950 no . . C(21) H(20) 0.950 no . . C(22) H(21) 0.950 no . . C(24) H(22) 0.950 no . . C(25) H(23) 0.950 no . . C(26) H(24) 0.950 no . . C(27) H(25) 0.950 no . . C(28) H(26) 0.950 no . . C(30) H(27) 0.950 no . . C(31) H(28) 0.950 no . . C(32) H(29) 0.950 no . . C(33) H(30) 0.950 no . . C(34) H(31) 0.950 no . . C(36) H(32) 0.950 no . . C(37) H(33) 0.950 no . . C(38) H(34) 0.950 no . . C(39) H(35) 0.950 no . . C(40) H(36) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Cu(1) Cl(3) 102.97(11) yes . . 3_555 Cl(1) Cu(1) P(1) 124.43(12) yes . . . Cl(3) Cu(1) P(1) 132.05(13) yes 3_555 . . Cl(1) Cu(2) Cl(2) 95.67(11) yes . . . Cl(1) Cu(2) Cl(2) 94.34(9) yes . . 3_555 Cl(1) Cu(2) P(2) 125.37(11) yes . . . Cl(2) Cu(2) Cl(2) 91.14(9) yes . . 3_555 Cl(2) Cu(2) P(2) 132.88(12) yes . . . Cl(2) Cu(2) P(2) 105.92(10) yes 3_555 . . Cl(1) Cu(3) Cl(2) 103.02(10) yes 3_555 . . Cl(1) Cu(3) Cl(3) 92.96(10) yes 3_555 . . Cl(1) Cu(3) P(3) 113.83(11) yes 3_555 . . Cl(2) Cu(3) Cl(3) 96.69(11) yes . . . Cl(2) Cu(3) P(3) 130.21(11) yes . . . Cl(3) Cu(3) P(3) 112.92(11) yes . . . Cl(3) Cu(4) P(4) 129.52(12) yes . . . Cl(3) Cu(4) O(1) 100.8(2) yes . . . P(4) Cu(4) O(1) 129.5(2) yes . . . Cu(1) Cl(1) Cu(2) 80.60(10) yes . . . Cu(1) Cl(1) Cu(3) 74.44(10) yes . . 3_555 Cu(2) Cl(1) Cu(3) 80.94(9) yes . . 3_555 Cu(2) Cl(2) Cu(2) 88.86(10) yes . . 3_555 Cu(2) Cl(2) Cu(3) 83.86(10) yes . . . Cu(2) Cl(2) Cu(3) 79.21(9) yes 3_555 . . Cu(1) Cl(3) Cu(3) 73.60(9) yes 3_555 . . Cu(1) Cl(3) Cu(4) 80.88(10) yes 3_555 . . Cu(3) Cl(3) Cu(4) 77.26(10) yes . . . O(1) S(1) O(2) 120.2(5) yes . . . O(1) S(1) O(3) 110.3(6) yes . . . O(1) S(1) C(4) 103.7(7) yes . . . O(2) S(1) O(3) 115.9(7) yes . . . O(2) S(1) C(4) 101.6(7) yes . . . O(3) S(1) C(4) 102.2(8) yes . . . Cu(1) P(1) C(3) 110.8(3) yes . . . Cu(1) P(1) C(29) 115.9(3) yes . . . Cu(1) P(1) C(35) 113.1(3) yes . . . C(3) P(1) C(29) 106.1(4) yes . . . C(3) P(1) C(35) 103.8(4) yes . . . C(29) P(1) C(35) 106.1(4) yes . . . Cu(2) P(2) C(2) 112.2(3) yes . . . Cu(2) P(2) C(3) 113.7(3) yes . . . Cu(2) P(2) C(23) 119.6(3) yes . . . C(2) P(2) C(3) 101.6(4) yes . . . C(2) P(2) C(23) 104.0(4) yes . . . C(3) P(2) C(23) 103.7(4) yes . . . Cu(3) P(3) C(1) 116.3(3) yes . . . Cu(3) P(3) C(2) 114.9(3) yes . . . Cu(3) P(3) C(17) 112.5(3) yes . . . C(1) P(3) C(2) 98.0(4) yes . . . C(1) P(3) C(17) 106.6(4) yes . . . C(2) P(3) C(17) 107.2(4) yes . . . Cu(4) P(4) C(1) 113.6(3) yes . . . Cu(4) P(4) C(5) 115.8(3) yes . . . Cu(4) P(4) C(11) 114.4(3) yes . . . C(1) P(4) C(5) 100.8(4) yes . . . C(1) P(4) C(11) 106.1(4) yes . . . C(5) P(4) C(11) 104.7(4) yes . . . Cu(4) O(1) S(1) 104.0(4) yes . . . P(3) C(1) P(4) 114.3(5) yes . . . P(2) C(2) P(3) 114.3(5) yes . . . P(1) C(3) P(2) 113.8(5) yes . . . S(1) C(4) F(1) 111.2(12) yes . . . S(1) C(4) F(2) 109.8(12) yes . . . S(1) C(4) F(3) 113.8(12) yes . . . F(1) C(4) F(2) 108.0(14) yes . . . F(1) C(4) F(3) 106.6(14) yes . . . F(2) C(4) F(3) 107.2(14) yes . . . P(4) C(5) C(6) 120.2(8) yes . . . P(4) C(5) C(10) 123.7(8) yes . . . C(6) C(5) C(10) 116.1(10) yes . . . C(5) C(6) C(7) 120.1(10) yes . . . C(6) C(7) C(8) 120.4(11) yes . . . C(7) C(8) C(9) 123.5(13) yes . . . C(8) C(9) C(10) 115.8(11) yes . . . C(5) C(10) C(9) 124.0(10) yes . . . P(4) C(11) C(12) 123.2(8) yes . . . P(4) C(11) C(16) 117.7(8) yes . . . C(12) C(11) C(16) 119.1(10) yes . . . C(11) C(12) C(13) 121.3(10) yes . . . C(12) C(13) C(14) 116.7(11) yes . . . C(13) C(14) C(15) 122.7(11) yes . . . C(14) C(15) C(16) 118.4(11) yes . . . C(11) C(16) C(15) 121.6(10) yes . . . P(3) C(17) C(18) 121.3(8) yes . . . P(3) C(17) C(22) 118.3(7) yes . . . C(18) C(17) C(22) 120.4(9) yes . . . C(17) C(18) C(19) 116.9(10) yes . . . C(18) C(19) C(20) 121.5(10) yes . . . C(19) C(20) C(21) 120.2(11) yes . . . C(20) C(21) C(22) 121.2(11) yes . . . C(17) C(22) C(21) 119.7(10) yes . . . P(2) C(23) C(24) 121.8(7) yes . . . P(2) C(23) C(28) 119.0(7) yes . . . C(24) C(23) C(28) 119.1(8) yes . . . C(23) C(24) C(25) 119.7(10) yes . . . C(24) C(25) C(26) 119.6(10) yes . . . C(25) C(26) C(27) 121.2(10) yes . . . C(26) C(27) C(28) 118.7(10) yes . . . C(23) C(28) C(27) 121.7(9) yes . . . P(1) C(29) C(30) 122.7(8) yes . . . P(1) C(29) C(34) 118.3(7) yes . . . C(30) C(29) C(34) 119.0(9) yes . . . C(29) C(30) C(31) 119.3(10) yes . . . C(30) C(31) C(32) 121.3(10) yes . . . C(31) C(32) C(33) 118.5(11) yes . . . C(32) C(33) C(34) 122.0(11) yes . . . C(29) C(34) C(33) 119.8(10) yes . . . P(1) C(35) C(36) 117.6(8) yes . . . P(1) C(35) C(40) 125.1(8) yes . . . C(36) C(35) C(40) 117.0(10) yes . . . C(35) C(36) C(37) 120.8(11) yes . . . C(36) C(37) C(38) 118.9(11) yes . . . C(37) C(38) C(39) 121.4(12) yes . . . C(38) C(39) C(40) 118.0(11) yes . . . C(35) C(40) C(39) 123.9(11) yes . . . P(3) C(1) H(1) 108.3 no . . . P(3) C(1) H(2) 108.1 no . . . P(4) C(1) H(1) 108.3 no . . . P(4) C(1) H(2) 108.2 no . . . H(1) C(1) H(2) 109.5 no . . . P(2) C(2) H(3) 108.4 no . . . P(2) C(2) H(4) 107.9 no . . . P(3) C(2) H(3) 108.7 no . . . P(3) C(2) H(4) 108.0 no . . . H(3) C(2) H(4) 109.5 no . . . P(1) C(3) H(5) 109.3 no . . . P(1) C(3) H(6) 107.7 no . . . P(2) C(3) H(5) 108.9 no . . . P(2) C(3) H(6) 107.7 no . . . H(5) C(3) H(6) 109.5 no . . . C(5) C(6) H(7) 118.7 no . . . C(7) C(6) H(7) 121.2 no . . . C(6) C(7) H(8) 119.1 no . . . C(8) C(7) H(8) 120.6 no . . . C(7) C(8) H(9) 117.3 no . . . C(9) C(8) H(9) 119.2 no . . . C(8) C(9) H(10) 121.5 no . . . C(10) C(9) H(10) 122.7 no . . . C(5) C(10) H(11) 117.0 no . . . C(9) C(10) H(11) 119.0 no . . . C(11) C(12) H(12) 119.4 no . . . C(13) C(12) H(12) 119.3 no . . . C(12) C(13) H(13) 121.6 no . . . C(14) C(13) H(13) 121.7 no . . . C(13) C(14) H(14) 117.7 no . . . C(15) C(14) H(14) 119.6 no . . . C(14) C(15) H(15) 120.4 no . . . C(16) C(15) H(15) 121.2 no . . . C(11) C(16) H(16) 118.1 no . . . C(15) C(16) H(16) 120.3 no . . . C(17) C(18) H(17) 121.3 no . . . C(19) C(18) H(17) 121.7 no . . . C(18) C(19) H(18) 119.5 no . . . C(20) C(19) H(18) 119.0 no . . . C(19) C(20) H(19) 120.5 no . . . C(21) C(20) H(19) 119.3 no . . . C(20) C(21) H(20) 118.4 no . . . C(22) C(21) H(20) 120.4 no . . . C(17) C(22) H(21) 120.9 no . . . C(21) C(22) H(21) 119.4 no . . . C(23) C(24) H(22) 119.8 no . . . C(25) C(24) H(22) 120.5 no . . . C(24) C(25) H(23) 121.2 no . . . C(26) C(25) H(23) 119.2 no . . . C(25) C(26) H(24) 120.3 no . . . C(27) C(26) H(24) 118.6 no . . . C(26) C(27) H(25) 120.4 no . . . C(28) C(27) H(25) 120.9 no . . . C(23) C(28) H(26) 118.9 no . . . C(27) C(28) H(26) 119.4 no . . . C(29) C(30) H(27) 119.3 no . . . C(31) C(30) H(27) 121.5 no . . . C(30) C(31) H(28) 120.3 no . . . C(32) C(31) H(28) 118.4 no . . . C(31) C(32) H(29) 121.7 no . . . C(33) C(32) H(29) 119.8 no . . . C(32) C(33) H(30) 117.3 no . . . C(34) C(33) H(30) 120.7 no . . . C(29) C(34) H(31) 120.9 no . . . C(33) C(34) H(31) 119.3 no . . . C(35) C(36) H(32) 119.6 no . . . C(37) C(36) H(32) 119.5 no . . . C(36) C(37) H(33) 120.2 no . . . C(38) C(37) H(33) 120.8 no . . . C(37) C(38) H(34) 119.3 no . . . C(39) C(38) H(34) 119.3 no . . . C(38) C(39) H(35) 121.4 no . . . C(40) C(39) H(35) 120.6 no . . . C(35) C(40) H(36) 117.6 no . . . C(39) C(40) H(36) 118.5 no . . . #============================================================================== #============================================================================== data__compound3b-revised _database_code_depnum_ccdc_archive 'CCDC 731697' _audit_creation_date 2009-08-05 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C89.50 H106.50 Br4.80 Cu4 O5.75 P8 S5.75 ' _chemical_formula_moiety 'C89.50 H106.50 Br4.80 Cu4 O5.75 P8 S5.75 ' _chemical_formula_weight 2344.18 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.5897(8) _cell_length_b 20.9612(9) _cell_length_c 33.0596(13) _cell_angle_alpha 90.0000 _cell_angle_beta 90.3600(8) _cell_angle_gamma 90.0000 _cell_volume 10803.0(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 18993 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4742.00 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.428 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 64323 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.659 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.658 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 22846 _reflns_number_gt 16012 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.2897 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 22846 _refine_ls_number_parameters 1111 _refine_ls_goodness_of_fit_ref 1.390 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2130P)^2^+109.7027P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 2.35 _refine_diff_density_min -1.98 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Br Br -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.63725(6) -0.00328(4) 0.82925(3) 0.0372(2) Uani 1.00 1 d . . . Br(2) Br 0.57048(5) -0.01798(4) 0.70883(2) 0.0324(2) Uani 1.00 1 d . . . Br(3) Br 0.49506(6) 0.02461(4) 0.59595(2) 0.0344(2) Uani 1.00 1 d . . . Br(4) Br 0.3954(4) 0.1196(3) 0.5109(2) 0.0667(19) Uani 0.248(5) 1 d P . . Br(5) Br 1.1629(2) 0.24977(16) 0.73743(9) 0.0636(10) Uani 0.402(4) 1 d P A 1 Br(6) Br 1.0301(2) 0.27304(15) 0.71921(10) 0.0645(10) Uani 0.402(4) 1 d P A 1 Br(7) Br 0.8892(2) 0.3044(2) 0.70284(13) 0.0860(13) Uani 0.402(4) 1 d P A 1 Br(8) Br 0.9707(6) 0.3479(5) 0.5646(3) 0.116(4) Uani 0.199(6) 1 d P . . Br(9) Br 0.7924(10) 0.3415(8) 0.6158(6) 0.137(7) Uani 0.151(6) 1 d P . . Cu(1) Cu 0.66625(6) 0.10522(5) 0.85376(3) 0.0320(2) Uani 1.00 1 d . . . Cu(2) Cu 0.59883(6) 0.06259(5) 0.76476(3) 0.0289(2) Uani 1.00 1 d . . . Cu(3) Cu 0.52716(6) 0.07514(5) 0.66426(3) 0.0280(2) Uani 1.00 1 d . . . Cu(4) Cu 0.45621(7) 0.13558(5) 0.57812(3) 0.0345(2) Uani 1.00 1 d . . . S(1) S 0.74481(18) 0.05519(16) 0.94168(8) 0.0547(6) Uani 1.00 1 d . . . S(2) S 0.50345(19) 0.33830(12) 0.70510(8) 0.0480(6) Uani 1.00 1 d . . . S(3) S 0.2177(4) 0.2815(2) 0.86340(18) 0.1124(17) Uani 1.00 1 d . . . S(4) S 0.03688(18) 0.39455(16) 0.99847(10) 0.0597(7) Uani 1.00 1 d . . . S(5) S 0.0919(2) 0.44089(19) 0.44149(11) 0.0677(8) Uani 1.00 1 d . . . S(6) S 0.4372(3) 0.1027(2) 0.48441(13) 0.0726(13) Uani 0.752(5) 1 d P . . P(1) P 0.78589(13) 0.14726(12) 0.82787(6) 0.0320(4) Uani 1.00 1 d . . . P(2) P 0.71644(13) 0.11419(11) 0.74264(6) 0.0298(4) Uani 1.00 1 d . . . P(3) P 0.64725(13) 0.13161(11) 0.65394(6) 0.0286(4) Uani 1.00 1 d . . . P(4) P 0.57542(14) 0.19574(11) 0.57631(6) 0.0327(4) Uani 1.00 1 d . . . P(5) P 0.55010(13) 0.16733(10) 0.85942(6) 0.0255(4) Uani 1.00 1 d . . . P(6) P 0.47470(12) 0.11172(10) 0.77984(6) 0.0248(4) Uani 1.00 1 d . . . P(7) P 0.40497(13) 0.11156(10) 0.69081(6) 0.0253(4) Uani 1.00 1 d . . . P(8) P 0.33581(13) 0.16623(11) 0.60994(6) 0.0300(4) Uani 1.00 1 d . . . O(1) O 0.6934(5) 0.1023(3) 0.9191(2) 0.059(2) Uani 1.00 1 d . . . O(2) O 0.5209(6) 0.2699(4) 0.6943(2) 0.071(2) Uani 1.00 1 d . . . O(3) O 0.2311(9) 0.3056(7) 0.9065(4) 0.126(4) Uani 1.00 1 d . . . O(4) O -0.0066(4) 0.4190(4) 0.9613(2) 0.063(2) Uani 1.00 1 d . . . O(5) O 0.1325(5) 0.4483(5) 0.4830(3) 0.079(2) Uani 1.00 1 d . . . O(6) O 0.446(2) 0.1508(17) 0.5173(10) 0.096(8) Uiso 0.376(2) 1 d P B 2 O(7) O 0.374(2) 0.092(2) 0.5207(10) 0.132(17) Uiso 0.376(2) 1 d P B 2 C(1) C 0.7664(5) 0.1746(4) 0.7756(2) 0.0384(19) Uani 1.00 1 d . . . C(2) C 0.6993(5) 0.1676(4) 0.6988(2) 0.0328(17) Uani 1.00 1 d . . . C(3) C 0.6308(5) 0.2054(4) 0.6246(2) 0.0364(18) Uani 1.00 1 d . . . C(4) C 0.4916(4) 0.1820(3) 0.8122(2) 0.0274(15) Uani 1.00 1 d . . . C(5) C 0.4188(5) 0.1537(3) 0.7393(2) 0.0278(15) Uani 1.00 1 d . . . C(6) C 0.3509(5) 0.1776(4) 0.6642(2) 0.0323(17) Uani 1.00 1 d . . . C(11) C 0.7645(11) 0.0882(10) 0.9898(4) 0.105(6) Uani 1.00 1 d . . . C(12) C 0.6689(16) -0.0035(7) 0.9544(6) 0.125(8) Uani 1.00 1 d . . . C(13) C 0.5723(8) 0.3544(6) 0.7468(3) 0.061(2) Uani 1.00 1 d . . . C(14) C 0.4023(9) 0.3395(6) 0.7298(4) 0.075(4) Uani 1.00 1 d . . . C(15) C 0.2716(10) 0.3267(17) 0.8336(10) 0.193(17) Uani 1.00 1 d . . . C(16) C 0.1160(11) 0.3091(10) 0.8516(5) 0.104(5) Uani 1.00 1 d . . . C(17) C 0.0986(11) 0.3234(8) 0.9822(9) 0.136(9) Uani 1.00 1 d . . . C(18) C 0.1284(7) 0.4433(7) 1.0069(3) 0.069(3) Uani 1.00 1 d . . . C(19) C 0.0901(9) 0.3621(9) 0.4305(5) 0.094(5) Uani 1.00 1 d . . . C(20) C -0.0222(8) 0.4511(9) 0.4483(6) 0.098(5) Uani 1.00 1 d . . . C(21) C 0.4225(18) 0.1859(13) 0.4709(8) 0.049(6) Uiso 0.376(2) 1 d P B 2 C(22) C 0.3488(18) 0.0789(14) 0.4483(8) 0.049(6) Uiso 0.376(2) 1 d P B 2 C(23) C 0.404(3) 0.127(2) 0.4374(17) 0.108(15) Uiso 0.376(2) 1 d P B 2 C(24) C 0.370(2) 0.036(2) 0.4902(13) 0.082(10) Uiso 0.376(2) 1 d P B 2 C(101) C 0.8288(5) 0.2175(4) 0.8528(2) 0.039(2) Uani 1.00 1 d . . . C(102) C 0.8378(8) 0.2772(6) 0.8347(3) 0.062(3) Uani 1.00 1 d . . . C(103) C 0.8715(8) 0.3294(5) 0.8555(4) 0.067(3) Uani 1.00 1 d . . . C(104) C 0.8991(7) 0.3194(5) 0.8956(3) 0.058(2) Uani 1.00 1 d . . . C(105) C 0.8944(6) 0.2604(5) 0.9131(3) 0.049(2) Uani 1.00 1 d . . . C(106) C 0.8597(6) 0.2107(5) 0.8923(2) 0.042(2) Uani 1.00 1 d . . . C(107) C 0.8832(5) 0.0992(6) 0.8247(2) 0.047(2) Uani 1.00 1 d . . . C(108) C 0.8784(6) 0.0336(6) 0.8343(3) 0.056(2) Uani 1.00 1 d . . . C(109) C 0.9521(8) -0.0025(6) 0.8318(4) 0.069(3) Uani 1.00 1 d . . . C(110) C 1.0320(7) 0.0245(8) 0.8206(4) 0.076(4) Uani 1.00 1 d . . . C(111) C 1.0334(6) 0.0844(7) 0.8134(3) 0.063(3) Uani 1.00 1 d . . . C(112) C 0.9617(6) 0.1263(6) 0.8144(3) 0.054(2) Uani 1.00 1 d . . . C(113) C 0.8065(5) 0.0635(5) 0.7291(2) 0.043(2) Uani 1.00 1 d . . . C(114) C 0.8029(7) -0.0000(6) 0.7367(3) 0.057(2) Uani 1.00 1 d . . . C(115) C 0.8717(8) -0.0410(7) 0.7281(4) 0.075(4) Uani 1.00 1 d . . . C(116) C 0.9438(8) -0.0159(9) 0.7122(4) 0.081(5) Uani 1.00 1 d . . . C(117) C 0.9511(7) 0.0470(8) 0.7048(4) 0.072(3) Uani 1.00 1 d . . . C(118) C 0.8822(6) 0.0902(8) 0.7125(3) 0.066(3) Uani 1.00 1 d . . . C(119) C 0.7358(5) 0.0897(4) 0.6291(2) 0.0354(19) Uani 1.00 1 d . . . C(120) C 0.7330(6) 0.0252(5) 0.6256(2) 0.042(2) Uani 1.00 1 d . . . C(121) C 0.8004(7) -0.0065(6) 0.6066(3) 0.058(2) Uani 1.00 1 d . . . C(122) C 0.8694(6) 0.0255(7) 0.5917(3) 0.058(3) Uani 1.00 1 d . . . C(123) C 0.8718(6) 0.0916(7) 0.5955(3) 0.059(3) Uani 1.00 1 d . . . C(124) C 0.8067(6) 0.1240(6) 0.6147(3) 0.050(2) Uani 1.00 1 d . . . C(125) C 0.6614(5) 0.1698(5) 0.5429(2) 0.044(2) Uani 1.00 1 d . . . C(126) C 0.6631(7) 0.1090(6) 0.5278(3) 0.059(3) Uani 1.00 1 d . . . C(127) C 0.7309(9) 0.0883(8) 0.5063(3) 0.085(5) Uani 1.00 1 d . . . C(128) C 0.7968(9) 0.1227(10) 0.4969(3) 0.081(5) Uani 1.00 1 d . . . C(129) C 0.8010(7) 0.1853(12) 0.5108(3) 0.099(7) Uani 1.00 1 d . . . C(130) C 0.7313(6) 0.2120(7) 0.5339(3) 0.062(3) Uani 1.00 1 d . . . C(131) C 0.5545(5) 0.2775(4) 0.5612(2) 0.0374(19) Uani 1.00 1 d . . . C(132) C 0.5569(7) 0.2943(5) 0.5192(2) 0.049(2) Uani 1.00 1 d . . . C(133) C 0.5319(9) 0.3536(6) 0.5069(3) 0.067(3) Uani 1.00 1 d . . . C(134) C 0.5075(8) 0.3990(5) 0.5346(4) 0.061(3) Uani 1.00 1 d . . . C(135) C 0.4980(12) 0.3823(7) 0.5738(4) 0.088(4) Uani 1.00 1 d . . . C(136) C 0.5271(10) 0.3216(6) 0.5867(3) 0.072(3) Uani 1.00 1 d . . . C(201) C 0.4658(5) 0.1415(4) 0.8936(2) 0.0313(17) Uani 1.00 1 d . . . C(202) C 0.4600(5) 0.0785(4) 0.9046(2) 0.0349(18) Uani 1.00 1 d . . . C(203) C 0.3923(6) 0.0591(4) 0.9304(3) 0.042(2) Uani 1.00 1 d . . . C(204) C 0.3358(6) 0.1006(5) 0.9443(2) 0.047(2) Uani 1.00 1 d . . . C(205) C 0.3411(6) 0.1646(5) 0.9330(3) 0.048(2) Uani 1.00 1 d . . . C(206) C 0.4047(5) 0.1857(4) 0.9085(2) 0.0366(18) Uani 1.00 1 d . . . C(207) C 0.5737(5) 0.2481(4) 0.8760(2) 0.0293(16) Uani 1.00 1 d . . . C(208) C 0.5367(6) 0.3025(4) 0.8593(2) 0.041(2) Uani 1.00 1 d . . . C(209) C 0.5595(7) 0.3635(4) 0.8732(3) 0.045(2) Uani 1.00 1 d . . . C(210) C 0.6210(6) 0.3687(5) 0.9037(3) 0.050(2) Uani 1.00 1 d . . . C(211) C 0.6573(7) 0.3158(6) 0.9202(4) 0.068(3) Uani 1.00 1 d . . . C(212) C 0.6355(6) 0.2554(4) 0.9066(3) 0.049(2) Uani 1.00 1 d . . . C(213) C 0.3903(5) 0.0680(4) 0.8062(2) 0.0314(17) Uani 1.00 1 d . . . C(214) C 0.4006(6) 0.0030(4) 0.8114(2) 0.0387(19) Uani 1.00 1 d . . . C(215) C 0.3373(7) -0.0304(5) 0.8317(3) 0.055(2) Uani 1.00 1 d . . . C(216) C 0.2684(6) -0.0023(6) 0.8472(3) 0.054(2) Uani 1.00 1 d . . . C(217) C 0.2584(5) 0.0640(5) 0.8428(3) 0.043(2) Uani 1.00 1 d . . . C(218) C 0.3182(5) 0.0979(5) 0.8217(2) 0.040(2) Uani 1.00 1 d . . . C(219) C 0.3212(5) 0.0534(4) 0.7014(2) 0.0316(17) Uani 1.00 1 d . . . C(220) C 0.2449(6) 0.0690(5) 0.7214(3) 0.045(2) Uani 1.00 1 d . . . C(221) C 0.1871(6) 0.0237(7) 0.7305(3) 0.062(3) Uani 1.00 1 d . . . C(222) C 0.2025(7) -0.0423(6) 0.7202(3) 0.058(2) Uani 1.00 1 d . . . C(223) C 0.2773(6) -0.0567(5) 0.6989(3) 0.047(2) Uani 1.00 1 d . . . C(224) C 0.3353(5) -0.0094(4) 0.6904(2) 0.0344(18) Uani 1.00 1 d . . . C(225) C 0.2429(5) 0.1129(4) 0.6090(2) 0.0347(18) Uani 1.00 1 d . . . C(226) C 0.1625(7) 0.1333(6) 0.6177(3) 0.058(2) Uani 1.00 1 d . . . C(227) C 0.0947(6) 0.0897(9) 0.6195(3) 0.079(4) Uani 1.00 1 d . . . C(228) C 0.1092(7) 0.0240(7) 0.6125(4) 0.065(3) Uani 1.00 1 d . . . C(229) C 0.1886(7) 0.0046(5) 0.6028(3) 0.057(2) Uani 1.00 1 d . . . C(230) C 0.2569(5) 0.0480(4) 0.6001(3) 0.040(2) Uani 1.00 1 d . . . C(231) C 0.2888(6) 0.2430(5) 0.5946(3) 0.047(2) Uani 1.00 1 d . . . C(232) C 0.2836(15) 0.2953(7) 0.6172(4) 0.116(8) Uani 1.00 1 d . . . C(233) C 0.2430(16) 0.3513(8) 0.6047(7) 0.128(8) Uani 1.00 1 d . . . C(234) C 0.2175(10) 0.3560(7) 0.5651(5) 0.079(4) Uani 1.00 1 d . . . C(235) C 0.2303(9) 0.3096(8) 0.5403(4) 0.084(4) Uani 1.00 1 d . . . C(236) C 0.2667(8) 0.2484(6) 0.5537(3) 0.065(3) Uani 1.00 1 d . . . H(1) H 0.7298 0.2115 0.7768 0.049 Uiso 1.00 1 c R . . H(2) H 0.8200 0.1875 0.7644 0.049 Uiso 1.00 1 c R . . H(3) H 0.6632 0.2017 0.7077 0.042 Uiso 1.00 1 c R . . H(4) H 0.7527 0.1837 0.6909 0.042 Uiso 1.00 1 c R . . H(5) H 0.5981 0.2341 0.6411 0.044 Uiso 1.00 1 c R . . H(6) H 0.6856 0.2240 0.6200 0.044 Uiso 1.00 1 c R . . H(7) H 0.4373 0.1999 0.8184 0.036 Uiso 1.00 1 c R . . H(8) H 0.5235 0.2131 0.7968 0.036 Uiso 1.00 1 c R . . H(9) H 0.3626 0.1646 0.7490 0.038 Uiso 1.00 1 c R . . H(10) H 0.4491 0.1925 0.7341 0.038 Uiso 1.00 1 c R . . H(11) H 0.2963 0.1831 0.6761 0.042 Uiso 1.00 1 c R . . H(12) H 0.3845 0.2149 0.6682 0.042 Uiso 1.00 1 c R . . H(13) H 0.7963 0.0584 1.0058 0.125 Uiso 1.00 1 c R . . H(14) H 0.7932 0.1266 0.9877 0.125 Uiso 1.00 1 c R . . H(15) H 0.7098 0.0948 1.0032 0.125 Uiso 1.00 1 c R . . H(16) H 0.6248 0.0147 0.9703 0.138 Uiso 1.00 1 c R . . H(17) H 0.6450 -0.0217 0.9306 0.138 Uiso 1.00 1 c R . . H(18) H 0.6966 -0.0366 0.9697 0.138 Uiso 1.00 1 c R . . H(19) H 0.5605 0.3253 0.7689 0.080 Uiso 1.00 1 c R . . H(20) H 0.6317 0.3477 0.7396 0.080 Uiso 1.00 1 c R . . H(21) H 0.5661 0.3965 0.7564 0.080 Uiso 1.00 1 c R . . H(22) H 0.3887 0.3820 0.7380 0.092 Uiso 1.00 1 c R . . H(23) H 0.3591 0.3232 0.7130 0.092 Uiso 1.00 1 c R . . H(24) H 0.4059 0.3137 0.7541 0.092 Uiso 1.00 1 c R . . H(25) H 0.3310 0.3182 0.8364 0.200 Uiso 1.00 1 c R . . H(26) H 0.2552 0.3169 0.8058 0.200 Uiso 1.00 1 c R . . H(27) H 0.2595 0.3695 0.8387 0.200 Uiso 1.00 1 c R . . H(28) H 0.1095 0.3526 0.8541 0.172 Uiso 1.00 1 c R . . H(29) H 0.1049 0.3004 0.8209 0.172 Uiso 1.00 1 c R . . H(30) H 0.0725 0.2858 0.8642 0.172 Uiso 1.00 1 c R . . H(31) H 0.0558 0.2954 0.9699 0.159 Uiso 1.00 1 c R . . H(32) H 0.1356 0.3375 0.9616 0.159 Uiso 1.00 1 c R . . H(33) H 0.1237 0.3061 1.0037 0.159 Uiso 1.00 1 c R . . H(34) H 0.1593 0.4293 1.0297 0.093 Uiso 1.00 1 c R . . H(35) H 0.1657 0.4406 0.9834 0.093 Uiso 1.00 1 c R . . H(36) H 0.1118 0.4865 1.0099 0.093 Uiso 1.00 1 c R . . H(37) H 0.0556 0.3382 0.4517 0.107 Uiso 1.00 1 c R . . H(38) H 0.0631 0.3518 0.4057 0.107 Uiso 1.00 1 c R . . H(39) H 0.1452 0.3422 0.4318 0.107 Uiso 1.00 1 c R . . H(40) H -0.0319 0.4941 0.4583 0.116 Uiso 1.00 1 c R . . H(41) H -0.0500 0.4480 0.4226 0.116 Uiso 1.00 1 c R . . H(42) H -0.0430 0.4217 0.4663 0.116 Uiso 1.00 1 c R . . H(43) H 0.8160 0.2844 0.8081 0.079 Uiso 1.00 1 c R . . H(44) H 0.8800 0.3707 0.8428 0.081 Uiso 1.00 1 c R . . H(45) H 0.9228 0.3550 0.9107 0.073 Uiso 1.00 1 c R . . H(46) H 0.9150 0.2544 0.9406 0.059 Uiso 1.00 1 c R . . H(47) H 0.8553 0.1701 0.9052 0.051 Uiso 1.00 1 c R . . H(48) H 0.8235 0.0147 0.8424 0.068 Uiso 1.00 1 c R . . H(49) H 0.9495 -0.0468 0.8395 0.078 Uiso 1.00 1 c R . . H(50) H 1.0796 -0.0048 0.8193 0.091 Uiso 1.00 1 c R . . H(51) H 1.0875 0.1017 0.8055 0.094 Uiso 1.00 1 c R . . H(52) H 0.9661 0.1714 0.8082 0.068 Uiso 1.00 1 c R . . H(53) H 0.7510 -0.0180 0.7479 0.067 Uiso 1.00 1 c R . . H(54) H 0.8673 -0.0866 0.7328 0.089 Uiso 1.00 1 c R . . H(55) H 0.9921 -0.0406 0.7058 0.114 Uiso 1.00 1 c R . . H(56) H 1.0017 0.0669 0.6920 0.088 Uiso 1.00 1 c R . . H(57) H 0.8861 0.1364 0.7078 0.076 Uiso 1.00 1 c R . . H(58) H 0.6854 0.0019 0.6360 0.053 Uiso 1.00 1 c R . . H(59) H 0.7976 -0.0533 0.6037 0.068 Uiso 1.00 1 c R . . H(60) H 0.9174 0.0065 0.5785 0.070 Uiso 1.00 1 c R . . H(61) H 0.9195 0.1130 0.5846 0.075 Uiso 1.00 1 c R . . H(62) H 0.8085 0.1695 0.6170 0.064 Uiso 1.00 1 c R . . H(63) H 0.6144 0.0794 0.5330 0.065 Uiso 1.00 1 c R . . H(64) H 0.7282 0.0442 0.4954 0.099 Uiso 1.00 1 c R . . H(65) H 0.8421 0.1032 0.4808 0.094 Uiso 1.00 1 c R . . H(66) H 0.8512 0.2115 0.5053 0.111 Uiso 1.00 1 c R . . H(67) H 0.7310 0.2556 0.5433 0.081 Uiso 1.00 1 c R . . H(68) H 0.5780 0.2640 0.5005 0.062 Uiso 1.00 1 c R . . H(69) H 0.5327 0.3637 0.4785 0.078 Uiso 1.00 1 c R . . H(70) H 0.4945 0.4421 0.5266 0.075 Uiso 1.00 1 c R . . H(71) H 0.4803 0.4137 0.5934 0.101 Uiso 1.00 1 c R . . H(72) H 0.5232 0.3110 0.6151 0.082 Uiso 1.00 1 c R . . H(73) H 0.5000 0.0474 0.8946 0.044 Uiso 1.00 1 c R . . H(74) H 0.3893 0.0160 0.9382 0.051 Uiso 1.00 1 c R . . H(75) H 0.2903 0.0861 0.9620 0.055 Uiso 1.00 1 c R . . H(76) H 0.2967 0.1923 0.9422 0.062 Uiso 1.00 1 c R . . H(77) H 0.4085 0.2303 0.9005 0.048 Uiso 1.00 1 c R . . H(78) H 0.4951 0.2974 0.8390 0.048 Uiso 1.00 1 c R . . H(79) H 0.5340 0.4010 0.8617 0.056 Uiso 1.00 1 c R . . H(80) H 0.6408 0.4098 0.9126 0.062 Uiso 1.00 1 c R . . H(81) H 0.6954 0.3201 0.9421 0.077 Uiso 1.00 1 c R . . H(82) H 0.6665 0.2194 0.9165 0.062 Uiso 1.00 1 c R . . H(83) H 0.4486 -0.0188 0.7999 0.049 Uiso 1.00 1 c R . . H(84) H 0.3440 -0.0768 0.8352 0.066 Uiso 1.00 1 c R . . H(85) H 0.2246 -0.0265 0.8607 0.069 Uiso 1.00 1 c R . . H(86) H 0.2113 0.0839 0.8553 0.056 Uiso 1.00 1 c R . . H(87) H 0.3106 0.1431 0.8176 0.051 Uiso 1.00 1 c R . . H(88) H 0.2344 0.1130 0.7279 0.054 Uiso 1.00 1 c R . . H(89) H 0.1344 0.0353 0.7439 0.070 Uiso 1.00 1 c R . . H(90) H 0.1623 -0.0754 0.7278 0.073 Uiso 1.00 1 c R . . H(91) H 0.2868 -0.0987 0.6886 0.054 Uiso 1.00 1 c R . . H(92) H 0.3872 -0.0208 0.6771 0.043 Uiso 1.00 1 c R . . H(93) H 0.1530 0.1768 0.6222 0.065 Uiso 1.00 1 c R . . H(94) H 0.0393 0.1056 0.6272 0.084 Uiso 1.00 1 c R . . H(95) H 0.0633 -0.0051 0.6137 0.077 Uiso 1.00 1 c R . . H(96) H 0.1990 -0.0388 0.5975 0.068 Uiso 1.00 1 c R . . H(97) H 0.3123 0.0348 0.5920 0.050 Uiso 1.00 1 c R . . H(98) H 0.3007 0.2901 0.6455 0.194 Uiso 1.00 1 c R . . H(99) H 0.2388 0.3878 0.6235 0.158 Uiso 1.00 1 c R . . H(100) H 0.1879 0.3928 0.5546 0.101 Uiso 1.00 1 c R . . H(101) H 0.2121 0.3114 0.5117 0.096 Uiso 1.00 1 c R . . H(102) H 0.2759 0.2138 0.5359 0.080 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0427(4) 0.0344(4) 0.0344(4) 0.0034(3) -0.0095(3) 0.0032(3) Br(2) 0.0367(4) 0.0303(4) 0.0300(4) 0.0030(3) -0.0080(3) 0.0011(3) Br(3) 0.0421(4) 0.0307(4) 0.0304(4) -0.0006(3) -0.0063(3) -0.0047(3) Br(4) 0.068(3) 0.065(3) 0.067(3) -0.001(2) -0.008(2) -0.014(2) Br(5) 0.076(2) 0.067(2) 0.0478(15) -0.0121(14) 0.0216(13) -0.0259(13) Br(6) 0.079(2) 0.0567(18) 0.0575(17) -0.0179(15) 0.0105(14) -0.0053(13) Br(7) 0.079(2) 0.093(2) 0.086(2) -0.042(2) 0.0147(19) 0.023(2) Br(8) 0.092(6) 0.129(9) 0.127(8) 0.008(5) -0.008(5) 0.045(6) Br(9) 0.111(11) 0.113(11) 0.187(18) -0.017(8) 0.029(10) -0.040(10) Cu(1) 0.0299(5) 0.0384(5) 0.0275(5) 0.0049(4) -0.0041(3) 0.0012(4) Cu(2) 0.0254(4) 0.0337(5) 0.0276(4) 0.0032(3) -0.0028(3) -0.0001(3) Cu(3) 0.0274(4) 0.0308(5) 0.0256(4) 0.0002(3) -0.0044(3) -0.0006(3) Cu(4) 0.0364(5) 0.0335(5) 0.0335(5) -0.0036(4) -0.0032(4) -0.0008(4) S(1) 0.0530(14) 0.0716(19) 0.0394(12) 0.0161(13) -0.0016(11) 0.0052(12) S(2) 0.0696(16) 0.0344(12) 0.0399(12) -0.0099(11) -0.0004(11) -0.0014(9) S(3) 0.135(4) 0.098(3) 0.104(3) 0.020(3) -0.043(3) -0.006(2) S(4) 0.0454(14) 0.0723(19) 0.0612(17) -0.0108(13) -0.0082(12) 0.0117(14) S(5) 0.0501(15) 0.087(2) 0.0660(19) -0.0058(15) -0.0039(14) 0.0025(17) S(6) 0.090(3) 0.080(3) 0.048(2) 0.005(2) -0.003(2) -0.012(2) P(1) 0.0271(10) 0.0451(12) 0.0239(9) 0.0012(8) -0.0076(7) -0.0023(8) P(2) 0.0236(9) 0.0443(12) 0.0215(9) -0.0018(8) -0.0059(7) -0.0008(8) P(3) 0.0272(9) 0.0371(11) 0.0215(9) -0.0012(8) -0.0059(7) 0.0014(8) P(4) 0.0323(10) 0.0389(12) 0.0269(10) -0.0046(8) -0.0032(8) 0.0078(8) P(5) 0.0281(9) 0.0295(10) 0.0189(8) 0.0004(7) -0.0062(7) -0.0014(7) P(6) 0.0237(9) 0.0303(10) 0.0203(8) 0.0026(7) -0.0068(6) -0.0031(7) P(7) 0.0274(9) 0.0273(10) 0.0210(8) 0.0025(7) -0.0089(7) -0.0031(7) P(8) 0.0306(10) 0.0354(11) 0.0239(9) 0.0003(8) -0.0118(7) -0.0007(8) O(1) 0.097(6) 0.049(4) 0.030(3) 0.008(4) -0.013(3) -0.002(3) O(2) 0.085(5) 0.053(4) 0.075(5) -0.012(4) 0.029(4) -0.029(4) O(3) 0.154(12) 0.120(10) 0.105(9) 0.014(9) -0.053(9) 0.006(8) O(4) 0.039(3) 0.088(6) 0.062(4) -0.009(3) -0.023(3) 0.002(4) O(5) 0.062(5) 0.099(7) 0.076(6) 0.011(4) -0.015(4) -0.020(5) C(1) 0.038(4) 0.051(5) 0.026(4) -0.007(3) -0.011(3) 0.001(3) C(2) 0.029(3) 0.043(4) 0.026(3) -0.001(3) -0.009(3) -0.003(3) C(3) 0.038(4) 0.045(5) 0.025(3) -0.009(3) -0.004(3) 0.006(3) C(4) 0.026(3) 0.032(4) 0.024(3) 0.002(3) -0.010(2) -0.003(3) C(5) 0.037(4) 0.030(4) 0.016(3) 0.006(3) -0.008(2) -0.005(2) C(6) 0.033(4) 0.036(4) 0.028(3) 0.009(3) -0.014(3) -0.000(3) C(11) 0.113(12) 0.149(16) 0.052(7) 0.057(11) -0.048(8) -0.039(9) C(12) 0.20(2) 0.050(8) 0.126(16) -0.008(11) 0.059(15) 0.021(9) C(13) 0.068(7) 0.068(7) 0.047(6) 0.010(6) -0.008(5) -0.004(5) C(14) 0.087(9) 0.049(6) 0.089(9) -0.011(6) 0.025(7) -0.033(6) C(15) 0.031(7) 0.30(3) 0.25(3) -0.009(13) 0.005(12) -0.16(3) C(16) 0.088(11) 0.139(16) 0.085(11) -0.004(10) 0.010(8) 0.021(11) C(17) 0.082(11) 0.063(10) 0.26(2) 0.004(8) -0.037(14) -0.052(14) C(18) 0.057(6) 0.093(9) 0.055(6) -0.021(6) -0.027(5) -0.003(6) C(19) 0.055(7) 0.119(13) 0.107(12) 0.005(8) -0.025(7) -0.050(10) C(20) 0.042(6) 0.118(14) 0.133(15) 0.012(7) -0.014(8) 0.025(11) C(101) 0.034(4) 0.053(5) 0.028(4) 0.010(3) -0.017(3) -0.008(3) C(102) 0.081(8) 0.059(7) 0.046(5) -0.010(6) -0.033(5) 0.001(5) C(103) 0.076(8) 0.038(5) 0.085(9) 0.002(5) -0.038(6) -0.009(5) C(104) 0.051(6) 0.057(7) 0.065(7) 0.001(5) -0.026(5) -0.020(5) C(105) 0.045(5) 0.064(6) 0.037(4) -0.005(4) -0.019(4) -0.005(4) C(106) 0.046(5) 0.058(6) 0.022(3) 0.009(4) -0.010(3) -0.008(3) C(107) 0.027(4) 0.083(7) 0.031(4) 0.009(4) -0.014(3) -0.015(4) C(108) 0.041(5) 0.066(7) 0.061(6) 0.011(5) -0.016(4) -0.008(5) C(109) 0.061(7) 0.072(8) 0.074(8) 0.026(6) -0.014(6) -0.010(6) C(110) 0.047(6) 0.109(12) 0.073(8) 0.041(7) -0.024(5) -0.034(8) C(111) 0.033(5) 0.098(10) 0.059(6) 0.017(5) -0.003(4) -0.009(6) C(112) 0.037(5) 0.071(7) 0.053(6) 0.000(4) 0.002(4) -0.011(5) C(113) 0.030(4) 0.075(7) 0.023(3) 0.004(4) -0.007(3) -0.005(4) C(114) 0.060(6) 0.061(7) 0.049(6) 0.026(5) -0.021(5) -0.011(5) C(115) 0.058(7) 0.105(11) 0.063(7) 0.041(7) -0.020(6) -0.018(7) C(116) 0.044(6) 0.141(15) 0.059(7) 0.047(8) -0.012(5) -0.021(8) C(117) 0.034(5) 0.113(12) 0.068(8) 0.013(6) 0.018(5) 0.001(8) C(118) 0.031(4) 0.128(12) 0.040(5) -0.000(6) 0.003(4) -0.001(6) C(119) 0.030(4) 0.057(5) 0.019(3) -0.004(3) -0.006(3) 0.001(3) C(120) 0.043(4) 0.051(5) 0.032(4) 0.003(4) -0.002(3) -0.010(4) C(121) 0.055(6) 0.080(8) 0.038(5) 0.021(5) -0.003(4) -0.012(5) C(122) 0.035(5) 0.107(10) 0.032(4) 0.016(5) -0.002(3) -0.001(5) C(123) 0.029(4) 0.107(10) 0.042(5) 0.008(5) 0.003(4) 0.010(6) C(124) 0.031(4) 0.083(7) 0.036(4) 0.006(4) -0.001(3) 0.011(4) C(125) 0.033(4) 0.072(7) 0.028(4) 0.007(4) -0.003(3) 0.013(4) C(126) 0.052(5) 0.083(8) 0.042(5) 0.024(5) 0.012(4) 0.031(5) C(127) 0.072(8) 0.129(13) 0.055(7) 0.063(8) 0.026(6) 0.048(8) C(128) 0.054(7) 0.151(15) 0.037(6) 0.044(9) -0.000(5) 0.005(8) C(129) 0.033(5) 0.23(2) 0.031(5) -0.006(9) -0.008(4) 0.046(9) C(130) 0.038(5) 0.121(11) 0.028(4) -0.010(6) -0.008(3) 0.012(5) C(131) 0.035(4) 0.042(5) 0.035(4) -0.015(3) -0.007(3) 0.008(3) C(132) 0.070(6) 0.049(5) 0.029(4) -0.005(5) -0.017(4) 0.001(4) C(133) 0.106(9) 0.056(7) 0.038(5) -0.027(6) -0.031(6) 0.021(5) C(134) 0.068(7) 0.040(5) 0.074(8) -0.000(5) -0.013(6) 0.022(5) C(135) 0.135(14) 0.067(9) 0.062(8) 0.043(9) -0.003(8) 0.004(6) C(136) 0.114(11) 0.064(8) 0.037(5) 0.021(7) 0.011(6) 0.012(5) C(201) 0.028(3) 0.045(4) 0.021(3) -0.005(3) -0.007(2) -0.002(3) C(202) 0.038(4) 0.042(4) 0.025(3) 0.001(3) -0.008(3) 0.000(3) C(203) 0.041(4) 0.040(5) 0.044(5) -0.010(3) -0.006(3) 0.000(4) C(204) 0.037(4) 0.068(6) 0.036(4) 0.002(4) -0.001(3) 0.004(4) C(205) 0.041(5) 0.063(6) 0.042(5) 0.002(4) 0.009(4) -0.001(4) C(206) 0.032(4) 0.045(5) 0.033(4) 0.005(3) -0.001(3) -0.001(3) C(207) 0.032(3) 0.034(4) 0.023(3) 0.002(3) -0.010(3) -0.004(3) C(208) 0.052(5) 0.036(4) 0.034(4) -0.000(4) -0.014(3) -0.001(3) C(209) 0.062(6) 0.036(5) 0.037(4) -0.003(4) -0.007(4) -0.002(3) C(210) 0.054(5) 0.041(5) 0.057(6) 0.006(4) -0.017(4) -0.023(4) C(211) 0.054(6) 0.069(7) 0.081(8) 0.007(5) -0.040(6) -0.046(6) C(212) 0.056(5) 0.038(5) 0.052(5) 0.012(4) -0.029(4) -0.019(4) C(213) 0.028(3) 0.039(4) 0.027(3) -0.000(3) -0.008(3) -0.008(3) C(214) 0.045(4) 0.028(4) 0.044(4) -0.001(3) 0.001(3) -0.001(3) C(215) 0.053(6) 0.052(6) 0.060(6) -0.014(5) 0.013(5) 0.002(5) C(216) 0.033(4) 0.073(7) 0.056(6) -0.012(4) -0.000(4) 0.005(5) C(217) 0.032(4) 0.057(6) 0.042(5) -0.009(4) -0.000(3) -0.007(4) C(218) 0.026(4) 0.056(5) 0.037(4) 0.007(3) -0.003(3) -0.011(4) C(219) 0.032(3) 0.043(4) 0.020(3) -0.002(3) -0.006(2) -0.005(3) C(220) 0.033(4) 0.056(6) 0.046(5) -0.008(4) -0.004(3) -0.015(4) C(221) 0.037(5) 0.103(10) 0.047(6) -0.010(5) 0.016(4) -0.019(6) C(222) 0.054(6) 0.077(8) 0.042(5) -0.022(5) -0.009(4) -0.002(5) C(223) 0.040(4) 0.046(5) 0.054(5) -0.007(4) -0.013(4) 0.005(4) C(224) 0.030(4) 0.039(4) 0.034(4) -0.000(3) -0.008(3) 0.005(3) C(225) 0.037(4) 0.042(5) 0.025(3) -0.001(3) -0.013(3) 0.003(3) C(226) 0.055(6) 0.077(8) 0.043(5) 0.008(5) -0.017(4) -0.004(5) C(227) 0.025(4) 0.155(16) 0.056(7) -0.009(6) -0.005(4) 0.009(8) C(228) 0.042(5) 0.084(9) 0.067(7) -0.023(6) -0.022(5) 0.018(6) C(229) 0.060(6) 0.055(6) 0.056(6) -0.018(5) -0.018(5) 0.012(5) C(230) 0.029(4) 0.045(5) 0.047(5) -0.009(3) -0.009(3) 0.001(4) C(231) 0.047(5) 0.043(5) 0.052(5) 0.011(4) -0.013(4) 0.010(4) C(232) 0.21(2) 0.069(9) 0.067(9) 0.060(12) -0.074(11) -0.018(7) C(233) 0.19(2) 0.055(9) 0.134(16) 0.028(11) -0.081(15) 0.016(9) C(234) 0.099(10) 0.059(8) 0.078(9) 0.012(7) -0.009(8) 0.023(7) C(235) 0.075(8) 0.106(12) 0.072(9) 0.003(8) -0.029(7) 0.054(9) C(236) 0.088(8) 0.065(7) 0.041(5) 0.006(6) -0.016(5) 0.025(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Br(1) Cu(1) 2.4554(13) yes . . Br(1) Cu(2) 2.6066(13) yes . . Br(2) Cu(2) 2.5409(12) yes . . Br(2) Cu(3) 2.5347(12) yes . . Br(3) Cu(3) 2.5413(12) yes . . Br(3) Cu(4) 2.4739(13) yes . . Br(4) Cu(4) 2.433(6) yes . . Br(5) Br(6) 2.208(4) yes . . Br(6) Br(7) 2.352(5) yes . . Cu(1) P(1) 2.238(2) yes . . Cu(1) P(5) 2.239(2) yes . . Cu(1) O(1) 2.200(7) yes . . Cu(2) P(2) 2.255(2) yes . . Cu(2) P(6) 2.251(2) yes . . Cu(3) P(3) 2.243(2) yes . . Cu(3) P(7) 2.237(2) yes . . Cu(4) P(4) 2.247(2) yes . . Cu(4) P(8) 2.251(2) yes . . Cu(4) O(6) 2.04(3) yes . . Cu(4) O(7) 2.46(3) yes . . S(1) O(1) 1.472(8) yes . . S(1) C(11) 1.761(15) yes . . S(1) C(12) 1.76(2) yes . . S(2) O(2) 1.503(8) yes . . S(2) C(13) 1.774(12) yes . . S(2) C(14) 1.782(15) yes . . S(3) O(3) 1.526(15) yes . . S(3) C(15) 1.61(3) yes . . S(3) C(16) 1.729(19) yes . . S(4) O(4) 1.490(8) yes . . S(4) C(17) 1.857(19) yes . . S(4) C(18) 1.776(13) yes . . S(5) O(5) 1.515(10) yes . . S(5) C(19) 1.691(19) yes . . S(5) C(20) 1.806(13) yes . . S(6) O(6) 1.49(3) yes . . S(6) O(7) 1.57(3) yes . . S(6) C(21) 1.81(2) yes . . S(6) C(22) 1.88(2) yes . . S(6) C(23) 1.71(5) yes . . S(6) C(24) 1.76(4) yes . . P(1) C(1) 1.845(8) yes . . P(1) C(101) 1.813(10) yes . . P(1) C(107) 1.825(10) yes . . P(2) C(1) 1.839(9) yes . . P(2) C(2) 1.849(8) yes . . P(2) C(113) 1.819(10) yes . . P(3) C(2) 1.848(8) yes . . P(3) C(3) 1.843(9) yes . . P(3) C(119) 1.834(8) yes . . P(4) C(3) 1.820(8) yes . . P(4) C(125) 1.825(9) yes . . P(4) C(131) 1.815(9) yes . . P(5) C(4) 1.830(7) yes . . P(5) C(201) 1.822(8) yes . . P(5) C(207) 1.817(8) yes . . P(6) C(4) 1.839(8) yes . . P(6) C(5) 1.821(7) yes . . P(6) C(213) 1.830(8) yes . . P(7) C(5) 1.841(7) yes . . P(7) C(6) 1.841(8) yes . . P(7) C(219) 1.822(8) yes . . P(8) C(6) 1.822(8) yes . . P(8) C(225) 1.831(9) yes . . P(8) C(231) 1.838(10) yes . . C(101) C(102) 1.393(15) yes . . C(101) C(106) 1.398(12) yes . . C(102) C(103) 1.395(17) yes . . C(103) C(104) 1.407(18) yes . . C(104) C(105) 1.368(16) yes . . C(105) C(106) 1.359(15) yes . . C(107) C(108) 1.412(17) yes . . C(107) C(112) 1.394(14) yes . . C(108) C(109) 1.380(17) yes . . C(109) C(110) 1.420(18) yes . . C(110) C(111) 1.28(2) yes . . C(111) C(112) 1.421(17) yes . . C(113) C(114) 1.356(17) yes . . C(113) C(118) 1.420(14) yes . . C(114) C(115) 1.403(18) yes . . C(115) C(116) 1.351(19) yes . . C(116) C(117) 1.35(2) yes . . C(117) C(118) 1.429(19) yes . . C(119) C(120) 1.358(14) yes . . C(119) C(124) 1.405(13) yes . . C(120) C(121) 1.396(15) yes . . C(121) C(122) 1.363(16) yes . . C(122) C(123) 1.39(2) yes . . C(123) C(124) 1.381(15) yes . . C(125) C(126) 1.370(17) yes . . C(125) C(130) 1.436(16) yes . . C(126) C(127) 1.350(18) yes . . C(127) C(128) 1.29(2) yes . . C(128) C(129) 1.39(3) yes . . C(129) C(130) 1.445(18) yes . . C(131) C(132) 1.432(12) yes . . C(131) C(136) 1.324(16) yes . . C(132) C(133) 1.364(16) yes . . C(133) C(134) 1.374(17) yes . . C(134) C(135) 1.35(2) yes . . C(135) C(136) 1.42(2) yes . . C(201) C(202) 1.372(12) yes . . C(201) C(206) 1.419(12) yes . . C(202) C(203) 1.418(12) yes . . C(203) C(204) 1.322(14) yes . . C(204) C(205) 1.396(16) yes . . C(205) C(206) 1.359(13) yes . . C(207) C(208) 1.391(12) yes . . C(207) C(212) 1.400(13) yes . . C(208) C(209) 1.404(13) yes . . C(209) C(210) 1.390(15) yes . . C(210) C(211) 1.357(16) yes . . C(211) C(212) 1.386(16) yes . . C(213) C(214) 1.383(12) yes . . C(213) C(218) 1.387(12) yes . . C(214) C(215) 1.387(14) yes . . C(215) C(216) 1.331(15) yes . . C(216) C(217) 1.407(17) yes . . C(217) C(218) 1.366(13) yes . . C(219) C(220) 1.404(12) yes . . C(219) C(224) 1.383(12) yes . . C(220) C(221) 1.345(16) yes . . C(221) C(222) 1.445(19) yes . . C(222) C(223) 1.397(15) yes . . C(223) C(224) 1.374(13) yes . . C(225) C(226) 1.356(14) yes . . C(225) C(230) 1.408(13) yes . . C(226) C(227) 1.399(19) yes . . C(227) C(228) 1.42(2) yes . . C(228) C(229) 1.344(17) yes . . C(229) C(230) 1.403(15) yes . . C(231) C(232) 1.328(19) yes . . C(231) C(236) 1.398(15) yes . . C(232) C(233) 1.39(2) yes . . C(233) C(234) 1.37(2) yes . . C(234) C(235) 1.29(2) yes . . C(235) C(236) 1.47(2) yes . . C(1) H(1) 0.963 no . . C(1) H(2) 0.956 no . . C(2) H(3) 0.957 no . . C(2) H(4) 0.937 no . . C(3) H(5) 0.962 no . . C(3) H(6) 0.952 no . . C(4) H(7) 0.950 no . . C(4) H(8) 0.966 no . . C(5) H(9) 0.961 no . . C(5) H(10) 0.958 no . . C(6) H(11) 0.948 no . . C(6) H(12) 0.950 no . . C(11) H(13) 0.954 no . . C(11) H(14) 0.925 no . . C(11) H(15) 0.973 no . . C(12) H(16) 0.948 no . . C(12) H(17) 0.948 no . . C(12) H(18) 0.961 no . . C(13) H(19) 0.971 no . . C(13) H(20) 0.968 no . . C(13) H(21) 0.943 no . . C(14) H(22) 0.955 no . . C(14) H(23) 0.934 no . . C(14) H(24) 0.971 no . . C(15) H(25) 0.947 no . . C(15) H(26) 0.975 no . . C(15) H(27) 0.933 no . . C(16) H(28) 0.922 no . . C(16) H(29) 1.047 no . . C(16) H(30) 0.934 no . . C(17) H(31) 0.977 no . . C(17) H(32) 0.943 no . . C(17) H(33) 0.885 no . . C(18) H(34) 0.938 no . . C(18) H(35) 0.975 no . . C(18) H(36) 0.948 no . . C(19) H(37) 1.017 no . . C(19) H(38) 0.945 no . . C(19) H(39) 0.956 no . . C(20) H(40) 0.972 no . . C(20) H(41) 0.955 no . . C(20) H(42) 0.918 no . . C(102) H(43) 0.953 no . . C(103) H(44) 0.970 no . . C(104) H(45) 0.969 no . . C(105) H(46) 0.968 no . . C(106) H(47) 0.954 no . . C(108) H(48) 0.982 no . . C(109) H(49) 0.963 no . . C(110) H(50) 0.964 no . . C(111) H(51) 0.957 no . . C(112) H(52) 0.971 no . . C(114) H(53) 0.968 no . . C(115) H(54) 0.971 no . . C(116) H(55) 0.939 no . . C(117) H(56) 0.988 no . . C(118) H(57) 0.982 no . . C(120) H(58) 0.954 no . . C(121) H(59) 0.986 no . . C(122) H(60) 0.956 no . . C(123) H(61) 0.942 no . . C(124) H(62) 0.956 no . . C(126) H(63) 0.995 no . . C(127) H(64) 0.994 no . . C(128) H(65) 0.976 no . . C(129) H(66) 0.973 no . . C(130) H(67) 0.966 no . . C(132) H(68) 0.946 no . . C(133) H(69) 0.964 no . . C(134) H(70) 0.961 no . . C(135) H(71) 0.964 no . . C(136) H(72) 0.967 no . . C(202) H(73) 0.964 no . . C(203) H(74) 0.942 no . . C(204) H(75) 0.970 no . . C(205) H(76) 0.953 no . . C(206) H(77) 0.973 no . . C(208) H(78) 0.937 no . . C(209) H(79) 0.960 no . . C(210) H(80) 0.961 no . . C(211) H(81) 0.940 no . . C(212) H(82) 0.953 no . . C(214) H(83) 0.957 no . . C(215) H(84) 0.984 no . . C(216) H(85) 0.962 no . . C(217) H(86) 0.942 no . . C(218) H(87) 0.965 no . . C(220) H(88) 0.961 no . . C(221) H(89) 0.967 no . . C(222) H(90) 0.971 no . . C(223) H(91) 0.955 no . . C(224) H(92) 0.953 no . . C(226) H(93) 0.936 no . . C(227) H(94) 0.962 no . . C(228) H(95) 0.942 no . . C(229) H(96) 0.941 no . . C(230) H(97) 0.947 no . . C(232) H(98) 0.978 no . . C(233) H(99) 0.988 no . . C(234) H(100) 0.962 no . . C(235) H(101) 0.986 no . . C(236) H(102) 0.946 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) Br(1) Cu(2) 79.64(4) yes . . . Cu(2) Br(2) Cu(3) 87.46(4) yes . . . Cu(3) Br(3) Cu(4) 82.32(4) yes . . . Br(5) Br(6) Br(7) 175.8(2) yes . . . Br(1) Cu(1) P(1) 113.00(7) yes . . . Br(1) Cu(1) P(5) 114.76(6) yes . . . Br(1) Cu(1) O(1) 109.4(2) yes . . . P(1) Cu(1) P(5) 118.65(9) yes . . . P(1) Cu(1) O(1) 103.3(2) yes . . . P(5) Cu(1) O(1) 94.9(2) yes . . . Br(1) Cu(2) Br(2) 106.33(4) yes . . . Br(1) Cu(2) P(2) 109.65(6) yes . . . Br(1) Cu(2) P(6) 104.75(6) yes . . . Br(2) Cu(2) P(2) 102.76(6) yes . . . Br(2) Cu(2) P(6) 108.63(6) yes . . . P(2) Cu(2) P(6) 123.67(9) yes . . . Br(2) Cu(3) Br(3) 104.23(4) yes . . . Br(2) Cu(3) P(3) 105.98(6) yes . . . Br(2) Cu(3) P(7) 105.02(6) yes . . . Br(3) Cu(3) P(3) 104.16(6) yes . . . Br(3) Cu(3) P(7) 109.12(6) yes . . . P(3) Cu(3) P(7) 126.39(9) yes . . . Br(3) Cu(4) Br(4) 100.46(15) yes . . . Br(3) Cu(4) P(4) 109.43(7) yes . . . Br(3) Cu(4) P(8) 111.14(7) yes . . . Br(3) Cu(4) O(6) 113.6(9) yes . . . Br(3) Cu(4) O(7) 87.7(12) yes . . . Br(4) Cu(4) P(4) 111.75(16) yes . . . Br(4) Cu(4) P(8) 98.32(16) yes . . . Br(4) Cu(4) O(6) 24.9(9) yes . . . Br(4) Cu(4) O(7) 17.4(10) yes . . . P(4) Cu(4) P(8) 122.99(9) yes . . . P(4) Cu(4) O(6) 87.1(9) yes . . . P(4) Cu(4) O(7) 127.8(9) yes . . . P(8) Cu(4) O(6) 110.6(9) yes . . . P(8) Cu(4) O(7) 92.1(9) yes . . . O(1) S(1) C(11) 106.6(7) yes . . . O(1) S(1) C(12) 103.0(8) yes . . . C(11) S(1) C(12) 99.9(9) yes . . . O(2) S(2) C(13) 104.9(5) yes . . . O(2) S(2) C(14) 106.6(5) yes . . . C(13) S(2) C(14) 100.0(6) yes . . . O(3) S(3) C(15) 108.0(13) yes . . . O(3) S(3) C(16) 102.7(9) yes . . . C(15) S(3) C(16) 98.5(11) yes . . . O(4) S(4) C(17) 105.8(9) yes . . . O(4) S(4) C(18) 107.0(5) yes . . . C(17) S(4) C(18) 95.2(7) yes . . . O(5) S(5) C(19) 107.4(7) yes . . . O(5) S(5) C(20) 106.3(7) yes . . . C(19) S(5) C(20) 97.4(8) yes . . . O(6) S(6) C(23) 119(2) yes . . . O(6) S(6) C(24) 120.7(19) yes . . . O(7) S(6) C(21) 104(2) yes . . . O(7) S(6) C(22) 89.4(16) yes . . . C(21) S(6) C(22) 90.4(12) yes . . . C(23) S(6) C(24) 99(2) yes . . . Cu(1) P(1) C(1) 110.4(2) yes . . . Cu(1) P(1) C(101) 116.9(2) yes . . . Cu(1) P(1) C(107) 120.0(3) yes . . . C(1) P(1) C(101) 103.4(4) yes . . . C(1) P(1) C(107) 104.5(4) yes . . . C(101) P(1) C(107) 99.8(4) yes . . . Cu(2) P(2) C(1) 118.7(2) yes . . . Cu(2) P(2) C(2) 115.5(2) yes . . . Cu(2) P(2) C(113) 115.5(3) yes . . . C(1) P(2) C(2) 96.0(4) yes . . . C(1) P(2) C(113) 102.9(4) yes . . . C(2) P(2) C(113) 105.6(4) yes . . . Cu(3) P(3) C(2) 117.1(2) yes . . . Cu(3) P(3) C(3) 114.2(2) yes . . . Cu(3) P(3) C(119) 116.5(3) yes . . . C(2) P(3) C(3) 98.0(4) yes . . . C(2) P(3) C(119) 103.1(3) yes . . . C(3) P(3) C(119) 105.6(4) yes . . . Cu(4) P(4) C(3) 115.3(3) yes . . . Cu(4) P(4) C(125) 117.4(3) yes . . . Cu(4) P(4) C(131) 113.0(2) yes . . . C(3) P(4) C(125) 102.5(4) yes . . . C(3) P(4) C(131) 102.7(4) yes . . . C(125) P(4) C(131) 104.2(4) yes . . . Cu(1) P(5) C(4) 115.2(2) yes . . . Cu(1) P(5) C(201) 117.8(2) yes . . . Cu(1) P(5) C(207) 113.9(2) yes . . . C(4) P(5) C(201) 102.8(3) yes . . . C(4) P(5) C(207) 101.5(3) yes . . . C(201) P(5) C(207) 103.6(3) yes . . . Cu(2) P(6) C(4) 112.0(2) yes . . . Cu(2) P(6) C(5) 117.8(2) yes . . . Cu(2) P(6) C(213) 119.9(2) yes . . . C(4) P(6) C(5) 96.2(3) yes . . . C(4) P(6) C(213) 103.0(3) yes . . . C(5) P(6) C(213) 104.5(3) yes . . . Cu(3) P(7) C(5) 114.2(2) yes . . . Cu(3) P(7) C(6) 117.2(2) yes . . . Cu(3) P(7) C(219) 117.4(2) yes . . . C(5) P(7) C(6) 96.1(3) yes . . . C(5) P(7) C(219) 103.5(3) yes . . . C(6) P(7) C(219) 105.6(3) yes . . . Cu(4) P(8) C(6) 113.2(2) yes . . . Cu(4) P(8) C(225) 118.7(2) yes . . . Cu(4) P(8) C(231) 117.0(3) yes . . . C(6) P(8) C(225) 101.2(3) yes . . . C(6) P(8) C(231) 101.9(4) yes . . . C(225) P(8) C(231) 102.4(4) yes . . . Cu(1) O(1) S(1) 128.1(4) yes . . . Cu(4) O(6) S(6) 128(2) yes . . . Cu(4) O(7) S(6) 102(2) yes . . . P(1) C(1) P(2) 114.1(5) yes . . . P(2) C(2) P(3) 116.2(4) yes . . . P(3) C(3) P(4) 115.6(5) yes . . . P(5) C(4) P(6) 115.5(4) yes . . . P(6) C(5) P(7) 117.5(4) yes . . . P(7) C(6) P(8) 115.4(4) yes . . . Br(4) C(21) S(6) 35.2(5) yes . . . Br(4) C(21) O(6) 31.8(12) yes . . . Br(4) C(21) C(23) 84(2) yes . . . S(6) C(21) O(6) 49.5(14) yes . . . S(6) C(21) C(23) 58(2) yes . . . O(6) C(21) C(23) 108(2) yes . . . S(6) C(22) C(23) 61(2) yes . . . S(6) C(22) C(24) 58.8(17) yes . . . C(23) C(22) C(24) 119(3) yes . . . S(6) C(23) C(21) 65(2) yes . . . S(6) C(23) C(22) 74(2) yes . . . C(21) C(23) C(22) 118(4) yes . . . Br(4) C(24) S(6) 36.0(9) yes . . . Br(4) C(24) O(7) 21.2(16) yes . . . Br(4) C(24) C(22) 81(2) yes . . . S(6) C(24) O(7) 56(2) yes . . . S(6) C(24) C(22) 66.2(18) yes . . . O(7) C(24) C(22) 98(3) yes . . . P(1) C(101) C(102) 124.9(7) yes . . . P(1) C(101) C(106) 117.7(7) yes . . . C(102) C(101) C(106) 117.3(9) yes . . . C(101) C(102) C(103) 122.2(10) yes . . . C(102) C(103) C(104) 117.3(10) yes . . . C(103) C(104) C(105) 121.2(10) yes . . . C(104) C(105) C(106) 120.1(9) yes . . . C(101) C(106) C(105) 121.9(9) yes . . . P(1) C(107) C(108) 118.6(7) yes . . . P(1) C(107) C(112) 121.4(9) yes . . . C(108) C(107) C(112) 120.0(9) yes . . . C(107) C(108) C(109) 118.4(10) yes . . . C(108) C(109) C(110) 121.9(13) yes . . . C(109) C(110) C(111) 117.2(12) yes . . . C(110) C(111) C(112) 126.0(11) yes . . . C(107) C(112) C(111) 116.5(11) yes . . . P(2) C(113) C(114) 119.7(7) yes . . . P(2) C(113) C(118) 120.7(9) yes . . . C(114) C(113) C(118) 119.6(10) yes . . . C(113) C(114) C(115) 122.0(11) yes . . . C(114) C(115) C(116) 118.6(15) yes . . . C(115) C(116) C(117) 121.6(14) yes . . . C(116) C(117) C(118) 121.6(12) yes . . . C(113) C(118) C(117) 116.5(13) yes . . . P(3) C(119) C(120) 119.5(6) yes . . . P(3) C(119) C(124) 120.1(8) yes . . . C(120) C(119) C(124) 120.4(8) yes . . . C(119) C(120) C(121) 119.3(9) yes . . . C(120) C(121) C(122) 121.7(12) yes . . . C(121) C(122) C(123) 118.6(10) yes . . . C(122) C(123) C(124) 120.8(10) yes . . . C(119) C(124) C(123) 119.1(11) yes . . . P(4) C(125) C(126) 120.9(8) yes . . . P(4) C(125) C(130) 120.2(8) yes . . . C(126) C(125) C(130) 118.8(9) yes . . . C(125) C(126) C(127) 120.5(12) yes . . . C(126) C(127) C(128) 125.0(16) yes . . . C(127) C(128) C(129) 118.9(14) yes . . . C(128) C(129) C(130) 120.3(14) yes . . . C(125) C(130) C(129) 116.5(14) yes . . . P(4) C(131) C(132) 119.6(7) yes . . . P(4) C(131) C(136) 122.8(8) yes . . . C(132) C(131) C(136) 117.1(9) yes . . . C(131) C(132) C(133) 120.2(9) yes . . . C(132) C(133) C(134) 120.9(10) yes . . . C(133) C(134) C(135) 119.4(11) yes . . . C(134) C(135) C(136) 118.9(13) yes . . . C(131) C(136) C(135) 122.7(11) yes . . . P(5) C(201) C(202) 120.0(6) yes . . . P(5) C(201) C(206) 120.6(6) yes . . . C(202) C(201) C(206) 119.4(7) yes . . . C(201) C(202) C(203) 119.0(8) yes . . . C(202) C(203) C(204) 121.4(9) yes . . . C(203) C(204) C(205) 119.8(9) yes . . . C(204) C(205) C(206) 121.1(9) yes . . . C(201) C(206) C(205) 119.2(9) yes . . . P(5) C(207) C(208) 124.1(6) yes . . . P(5) C(207) C(212) 117.2(6) yes . . . C(208) C(207) C(212) 118.7(8) yes . . . C(207) C(208) C(209) 120.9(8) yes . . . C(208) C(209) C(210) 118.7(9) yes . . . C(209) C(210) C(211) 120.8(10) yes . . . C(210) C(211) C(212) 121.1(11) yes . . . C(207) C(212) C(211) 119.9(9) yes . . . P(6) C(213) C(214) 118.0(6) yes . . . P(6) C(213) C(218) 122.4(7) yes . . . C(214) C(213) C(218) 119.6(8) yes . . . C(213) C(214) C(215) 118.3(8) yes . . . C(214) C(215) C(216) 122.8(11) yes . . . C(215) C(216) C(217) 119.2(10) yes . . . C(216) C(217) C(218) 119.3(9) yes . . . C(213) C(218) C(217) 120.7(9) yes . . . P(7) C(219) C(220) 123.0(7) yes . . . P(7) C(219) C(224) 118.1(6) yes . . . C(220) C(219) C(224) 118.9(8) yes . . . C(219) C(220) C(221) 120.8(10) yes . . . C(220) C(221) C(222) 120.7(10) yes . . . C(221) C(222) C(223) 117.9(10) yes . . . C(222) C(223) C(224) 120.0(9) yes . . . C(219) C(224) C(223) 121.8(8) yes . . . P(8) C(225) C(226) 122.4(8) yes . . . P(8) C(225) C(230) 118.0(6) yes . . . C(226) C(225) C(230) 119.6(9) yes . . . C(225) C(226) C(227) 120.2(12) yes . . . C(226) C(227) C(228) 120.4(11) yes . . . C(227) C(228) C(229) 118.8(11) yes . . . C(228) C(229) C(230) 121.3(11) yes . . . C(225) C(230) C(229) 119.6(8) yes . . . P(8) C(231) C(232) 126.4(10) yes . . . P(8) C(231) C(236) 115.6(8) yes . . . C(232) C(231) C(236) 117.5(11) yes . . . C(231) C(232) C(233) 123.9(16) yes . . . C(232) C(233) C(234) 118.2(16) yes . . . C(233) C(234) C(235) 120.6(15) yes . . . C(234) C(235) C(236) 121.7(14) yes . . . C(231) C(236) C(235) 117.1(11) yes . . . P(1) C(1) H(1) 107.7 no . . . P(1) C(1) H(2) 108.1 no . . . P(2) C(1) H(1) 109.2 no . . . P(2) C(1) H(2) 109.6 no . . . H(1) C(1) H(2) 107.9 no . . . P(2) C(2) H(3) 107.2 no . . . P(2) C(2) H(4) 108.2 no . . . P(3) C(2) H(3) 107.1 no . . . P(3) C(2) H(4) 108.1 no . . . H(3) C(2) H(4) 110.0 no . . . P(3) C(3) H(5) 107.3 no . . . P(3) C(3) H(6) 107.8 no . . . P(4) C(3) H(5) 108.5 no . . . P(4) C(3) H(6) 109.1 no . . . H(5) C(3) H(6) 108.2 no . . . P(5) C(4) H(7) 108.8 no . . . P(5) C(4) H(8) 107.9 no . . . P(6) C(4) H(7) 108.6 no . . . P(6) C(4) H(8) 107.8 no . . . H(7) C(4) H(8) 108.1 no . . . P(6) C(5) H(9) 107.6 no . . . P(6) C(5) H(10) 107.9 no . . . P(7) C(5) H(9) 107.6 no . . . P(7) C(5) H(10) 107.9 no . . . H(9) C(5) H(10) 107.9 no . . . P(7) C(6) H(11) 107.6 no . . . P(7) C(6) H(12) 107.6 no . . . P(8) C(6) H(11) 108.4 no . . . P(8) C(6) H(12) 108.2 no . . . H(11) C(6) H(12) 109.6 no . . . S(1) C(11) H(13) 109.3 no . . . S(1) C(11) H(14) 110.8 no . . . S(1) C(11) H(15) 108.5 no . . . H(13) C(11) H(14) 111.3 no . . . H(13) C(11) H(15) 107.2 no . . . H(14) C(11) H(15) 109.7 no . . . S(1) C(12) H(16) 110.1 no . . . S(1) C(12) H(17) 110.2 no . . . S(1) C(12) H(18) 109.3 no . . . H(16) C(12) H(17) 109.8 no . . . H(16) C(12) H(18) 108.7 no . . . H(17) C(12) H(18) 108.7 no . . . S(2) C(13) H(19) 110.5 no . . . S(2) C(13) H(20) 110.9 no . . . S(2) C(13) H(21) 112.2 no . . . H(19) C(13) H(20) 106.3 no . . . H(19) C(13) H(21) 108.3 no . . . H(20) C(13) H(21) 108.5 no . . . S(2) C(14) H(22) 109.9 no . . . S(2) C(14) H(23) 111.0 no . . . S(2) C(14) H(24) 109.0 no . . . H(22) C(14) H(23) 110.5 no . . . H(22) C(14) H(24) 107.4 no . . . H(23) C(14) H(24) 109.0 no . . . S(3) C(15) H(25) 110.1 no . . . S(3) C(15) H(26) 108.6 no . . . S(3) C(15) H(27) 110.3 no . . . H(25) C(15) H(26) 107.6 no . . . H(25) C(15) H(27) 111.2 no . . . H(26) C(15) H(27) 108.8 no . . . S(3) C(16) H(28) 114.4 no . . . S(3) C(16) H(29) 107.9 no . . . S(3) C(16) H(30) 113.1 no . . . H(28) C(16) H(29) 103.8 no . . . H(28) C(16) H(30) 113.4 no . . . H(29) C(16) H(30) 102.9 no . . . S(4) C(17) H(31) 104.4 no . . . S(4) C(17) H(32) 106.1 no . . . S(4) C(17) H(33) 108.8 no . . . H(31) C(17) H(32) 107.8 no . . . H(31) C(17) H(33) 112.7 no . . . H(32) C(17) H(33) 116.1 no . . . S(4) C(18) H(34) 110.7 no . . . S(4) C(18) H(35) 108.9 no . . . S(4) C(18) H(36) 110.3 no . . . H(34) C(18) H(35) 108.4 no . . . H(34) C(18) H(36) 110.8 no . . . H(35) C(18) H(36) 107.6 no . . . S(5) C(19) H(37) 110.0 no . . . S(5) C(19) H(38) 114.5 no . . . S(5) C(19) H(39) 113.9 no . . . H(37) C(19) H(38) 104.4 no . . . H(37) C(19) H(39) 103.6 no . . . H(38) C(19) H(39) 109.4 no . . . S(5) C(20) H(40) 108.0 no . . . S(5) C(20) H(41) 108.7 no . . . S(5) C(20) H(42) 110.7 no . . . H(40) C(20) H(41) 107.2 no . . . H(40) C(20) H(42) 110.3 no . . . H(41) C(20) H(42) 111.8 no . . . C(101) C(102) H(43) 120.1 no . . . C(103) C(102) H(43) 117.5 no . . . C(102) C(103) H(44) 122.6 no . . . C(104) C(103) H(44) 120.0 no . . . C(103) C(104) H(45) 118.7 no . . . C(105) C(104) H(45) 120.1 no . . . C(104) C(105) H(46) 119.7 no . . . C(106) C(105) H(46) 120.2 no . . . C(101) C(106) H(47) 119.0 no . . . C(105) C(106) H(47) 119.1 no . . . C(107) C(108) H(48) 120.1 no . . . C(109) C(108) H(48) 121.5 no . . . C(108) C(109) H(49) 118.5 no . . . C(110) C(109) H(49) 119.5 no . . . C(109) C(110) H(50) 115.7 no . . . C(111) C(110) H(50) 127.2 no . . . C(110) C(111) H(51) 116.1 no . . . C(112) C(111) H(51) 117.8 no . . . C(107) C(112) H(52) 120.8 no . . . C(111) C(112) H(52) 122.7 no . . . C(113) C(114) H(53) 119.2 no . . . C(115) C(114) H(53) 118.7 no . . . C(114) C(115) H(54) 121.1 no . . . C(116) C(115) H(54) 120.3 no . . . C(115) C(116) H(55) 123.0 no . . . C(117) C(116) H(55) 115.4 no . . . C(116) C(117) H(56) 124.1 no . . . C(118) C(117) H(56) 114.2 no . . . C(113) C(118) H(57) 120.1 no . . . C(117) C(118) H(57) 123.4 no . . . C(119) C(120) H(58) 120.2 no . . . C(121) C(120) H(58) 120.5 no . . . C(120) C(121) H(59) 118.9 no . . . C(122) C(121) H(59) 119.3 no . . . C(121) C(122) H(60) 125.5 no . . . C(123) C(122) H(60) 115.9 no . . . C(122) C(123) H(61) 117.5 no . . . C(124) C(123) H(61) 121.7 no . . . C(119) C(124) H(62) 120.5 no . . . C(123) C(124) H(62) 120.4 no . . . C(125) C(126) H(63) 120.1 no . . . C(127) C(126) H(63) 119.5 no . . . C(126) C(127) H(64) 117.2 no . . . C(128) C(127) H(64) 117.6 no . . . C(127) C(128) H(65) 118.4 no . . . C(129) C(128) H(65) 122.7 no . . . C(128) C(129) H(66) 120.4 no . . . C(130) C(129) H(66) 119.3 no . . . C(125) C(130) H(67) 120.7 no . . . C(129) C(130) H(67) 122.8 no . . . C(131) C(132) H(68) 118.6 no . . . C(133) C(132) H(68) 121.2 no . . . C(132) C(133) H(69) 119.0 no . . . C(134) C(133) H(69) 120.1 no . . . C(133) C(134) H(70) 121.9 no . . . C(135) C(134) H(70) 118.7 no . . . C(134) C(135) H(71) 119.9 no . . . C(136) C(135) H(71) 120.4 no . . . C(131) C(136) H(72) 118.6 no . . . C(135) C(136) H(72) 118.5 no . . . C(201) C(202) H(73) 121.1 no . . . C(203) C(202) H(73) 119.9 no . . . C(202) C(203) H(74) 118.5 no . . . C(204) C(203) H(74) 120.1 no . . . C(203) C(204) H(75) 119.7 no . . . C(205) C(204) H(75) 120.5 no . . . C(204) C(205) H(76) 117.1 no . . . C(206) C(205) H(76) 121.7 no . . . C(201) C(206) H(77) 119.5 no . . . C(205) C(206) H(77) 121.3 no . . . C(207) C(208) H(78) 118.3 no . . . C(209) C(208) H(78) 120.8 no . . . C(208) C(209) H(79) 120.8 no . . . C(210) C(209) H(79) 120.5 no . . . C(209) C(210) H(80) 120.7 no . . . C(211) C(210) H(80) 118.4 no . . . C(210) C(211) H(81) 119.5 no . . . C(212) C(211) H(81) 119.3 no . . . C(207) C(212) H(82) 120.6 no . . . C(211) C(212) H(82) 119.3 no . . . C(213) C(214) H(83) 120.7 no . . . C(215) C(214) H(83) 120.9 no . . . C(214) C(215) H(84) 118.7 no . . . C(216) C(215) H(84) 118.5 no . . . C(215) C(216) H(85) 121.5 no . . . C(217) C(216) H(85) 119.3 no . . . C(216) C(217) H(86) 118.6 no . . . C(218) C(217) H(86) 122.0 no . . . C(213) C(218) H(87) 119.4 no . . . C(217) C(218) H(87) 119.8 no . . . C(219) C(220) H(88) 118.4 no . . . C(221) C(220) H(88) 120.8 no . . . C(220) C(221) H(89) 119.9 no . . . C(222) C(221) H(89) 119.5 no . . . C(221) C(222) H(90) 120.9 no . . . C(223) C(222) H(90) 121.2 no . . . C(222) C(223) H(91) 120.7 no . . . C(224) C(223) H(91) 119.2 no . . . C(219) C(224) H(92) 119.8 no . . . C(223) C(224) H(92) 118.4 no . . . C(225) C(226) H(93) 119.3 no . . . C(227) C(226) H(93) 120.5 no . . . C(226) C(227) H(94) 117.8 no . . . C(228) C(227) H(94) 121.7 no . . . C(227) C(228) H(95) 120.1 no . . . C(229) C(228) H(95) 121.0 no . . . C(228) C(229) H(96) 119.8 no . . . C(230) C(229) H(96) 118.9 no . . . C(225) C(230) H(97) 118.9 no . . . C(229) C(230) H(97) 121.5 no . . . C(231) C(232) H(98) 115.4 no . . . C(233) C(232) H(98) 119.8 no . . . C(232) C(233) H(99) 119.9 no . . . C(234) C(233) H(99) 121.6 no . . . C(233) C(234) H(100) 122.6 no . . . C(235) C(234) H(100) 116.7 no . . . C(234) C(235) H(101) 122.5 no . . . C(236) C(235) H(101) 115.5 no . . . C(231) C(236) H(102) 120.4 no . . . C(235) C(236) H(102) 122.6 no . . . #============================================================================== #============================================================================== data__compound4-revised #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731698' # CHEMICAL DATA _chemical_formula_sum 'C93 H107 Cl5 Cu5 N5 O5 P8 ' _chemical_formula_moiety 'C93 H107 Cl5 Cu5 N5 O5 P8 ' _chemical_formula_weight 2117.68 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 12.991(2) _cell_length_b 15.707(3) _cell_length_c 25.736(4) _cell_angle_alpha 102.7790(17) _cell_angle_beta 95.2180(18) _cell_angle_gamma 100.7290(11) _cell_volume 4983.9(14) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11547 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2180.00 _exptl_absorpt_coefficient_mu 1.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.711 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 43221 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 22348 _reflns_number_gt 17150 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1903 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 22348 _refine_ls_number_parameters 1136 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0522P)^2^+40.0734P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 1.75 _refine_diff_density_min -1.92 _refine_ls_extinction_method none _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.81173(5) 0.24555(4) 0.60898(3) 0.01946(14) Uani 1.00 1 d . . . Cu(2) Cu 0.87295(5) 0.45468(4) 0.65390(2) 0.01797(14) Uani 1.00 1 d . . . Cu(3) Cu 0.95918(5) 0.66381(4) 0.72985(2) 0.01806(14) Uani 1.00 1 d . . . Cu(4) Cu 1.05732(5) 0.83505(4) 0.82148(3) 0.02295(15) Uani 1.00 1 d . . . Cu(5) Cu 1.17716(8) 0.41741(7) 0.83412(4) 0.0484(2) Uani 1.00 1 d . . . Cl(1) Cl 0.76662(10) 0.35823(8) 0.57230(5) 0.0215(2) Uani 1.00 1 d . . . Cl(2) Cl 0.86175(10) 0.60052(8) 0.64247(5) 0.0209(2) Uani 1.00 1 d . . . Cl(3) Cl 0.96476(10) 0.82349(8) 0.73802(5) 0.0239(2) Uani 1.00 1 d . . . Cl(11) Cl 1.1093(2) 0.52205(17) 0.86996(10) 0.0648(6) Uani 1.00 1 d . . . Cl(12) Cl 1.2432(2) 0.31254(19) 0.79683(12) 0.0787(7) Uani 1.00 1 d . . . P(1) P 0.72585(10) 0.22477(8) 0.67768(5) 0.0175(2) Uani 1.00 1 d . . . P(2) P 0.78020(10) 0.42886(8) 0.72103(5) 0.0158(2) Uani 1.00 1 d . . . P(3) P 0.86168(10) 0.62180(8) 0.79096(5) 0.0166(2) Uani 1.00 1 d . . . P(4) P 0.96298(11) 0.78578(9) 0.88113(5) 0.0210(2) Uani 1.00 1 d . . . P(5) P 0.98402(10) 0.24030(8) 0.61493(5) 0.0166(2) Uani 1.00 1 d . . . P(6) P 1.04413(10) 0.44366(8) 0.65770(5) 0.0149(2) Uani 1.00 1 d . . . P(7) P 1.12265(10) 0.63863(8) 0.72674(5) 0.0148(2) Uani 1.00 1 d . . . P(8) P 1.21776(11) 0.80334(9) 0.81947(5) 0.0200(2) Uani 1.00 1 d . . . O(1) O 0.7562(4) 0.1301(3) 0.5426(2) 0.0444(11) Uani 1.00 1 d . . . O(2) O 1.0942(4) 0.9795(3) 0.8559(2) 0.0419(11) Uani 1.00 1 d . . . O(11) O 0.4588(9) 0.1962(7) 0.4799(5) 0.118(3) Uani 1.00 1 d D . . O(12) O 0.3723(11) 0.7137(8) 0.1574(5) 0.146(4) Uani 1.00 1 d D . . O(13) O 0.5905(9) 0.6899(8) 0.0200(4) 0.060(3) Uani 0.50 1 d PD . . O(14) O 0.2734(14) 0.4941(12) 0.0899(6) 0.094(4) Uani 0.50 1 d PD . . N(1) N 0.6546(5) 0.0409(4) 0.4679(2) 0.0463(14) Uani 1.00 1 d . . . N(2) N 1.0654(4) 1.1190(3) 0.8619(2) 0.0385(12) Uani 1.00 1 d . . . N(11) N 0.4287(5) 0.3084(5) 0.4450(3) 0.0550(16) Uani 1.00 1 d D . . N(12) N 0.5033(9) 0.8180(7) 0.1406(4) 0.088(2) Uani 1.00 1 d D . . N(13) N 0.4661(15) 0.5756(12) -0.0440(7) 0.080(5) Uani 0.50 1 d PD . . N(14) N 0.1312(16) 0.4911(14) 0.0318(8) 0.088(5) Uani 0.50 1 d PD . . C(1) C 0.7731(4) 0.3192(3) 0.7370(2) 0.0195(9) Uani 1.00 1 d . . . C(2) C 0.8324(4) 0.5011(3) 0.7884(2) 0.0184(9) Uani 1.00 1 d . . . C(3) C 0.9185(4) 0.6637(3) 0.8624(2) 0.0219(10) Uani 1.00 1 d . . . C(4) C 1.0683(4) 0.3350(3) 0.6664(2) 0.0172(9) Uani 1.00 1 d . . . C(5) C 1.1314(3) 0.5200(3) 0.7168(2) 0.0173(9) Uani 1.00 1 d . . . C(6) C 1.2155(3) 0.6850(3) 0.7896(2) 0.0176(9) Uani 1.00 1 d . . . C(11) C 0.6766(5) 0.1117(4) 0.5089(2) 0.0320(12) Uani 1.00 1 d . . . C(12) C 0.5595(7) 0.0191(6) 0.4289(4) 0.066(2) Uani 1.00 1 d . . . C(13) C 0.7276(13) -0.0175(11) 0.4589(6) 0.147(8) Uani 1.00 1 d . . . C(21) C 1.0538(5) 1.0336(4) 0.8373(2) 0.0358(13) Uani 1.00 1 d . . . C(22) C 1.0139(7) 1.1780(5) 0.8374(3) 0.056(2) Uani 1.00 1 d . . . C(23) C 1.1266(7) 1.1561(6) 0.9135(3) 0.064(2) Uani 1.00 1 d . . . C(31) C 0.4066(15) 0.2057(16) 0.4361(7) 0.157(8) Uani 1.00 1 d D . . C(32) C 0.3995(10) 0.3764(9) 0.4242(5) 0.089(3) Uani 1.00 1 d . . . C(33) C 0.5061(15) 0.3497(15) 0.4950(8) 0.144(6) Uani 1.00 1 d . . . C(34) C 0.4753(16) 0.7366(18) 0.1516(10) 0.174(9) Uani 1.00 1 d D . . C(35) C 0.4213(19) 0.8632(17) 0.1338(8) 0.158(7) Uani 1.00 1 d . . . C(36) C 0.6088(16) 0.8653(13) 0.1420(8) 0.141(6) Uani 1.00 1 d . . . C(37) C 0.5687(17) 0.6289(13) -0.0238(7) 0.073(5) Uani 0.50 1 d PD . . C(38) C 0.375(2) 0.589(2) -0.0052(13) 0.110(9) Uani 0.50 1 d P . . C(39) C 0.460(2) 0.4952(17) -0.0947(10) 0.098(8) Uani 0.50 1 d P . . C(40) C 0.1984(17) 0.5283(15) 0.0743(9) 0.076(5) Uani 0.50 1 d PD . . C(41) C 0.159(2) 0.408(2) -0.0043(12) 0.111(9) Uani 0.50 1 d P . . C(42) C 0.041(2) 0.530(2) 0.0204(15) 0.126(11) Uani 0.50 1 d P . . C(101) C 0.7465(4) 0.1283(3) 0.7025(2) 0.0232(10) Uani 1.00 1 d . . . C(102) C 0.7506(5) 0.1245(4) 0.7560(2) 0.0315(12) Uani 1.00 1 d . . . C(103) C 0.7659(5) 0.0470(4) 0.7711(2) 0.0393(15) Uani 1.00 1 d . . . C(104) C 0.7796(5) -0.0254(4) 0.7334(3) 0.0397(15) Uani 1.00 1 d . . . C(105) C 0.7778(6) -0.0221(5) 0.6801(3) 0.0471(17) Uani 1.00 1 d . . . C(106) C 0.7611(5) 0.0539(4) 0.6648(2) 0.0367(14) Uani 1.00 1 d . . . C(107) C 0.5822(4) 0.2124(3) 0.6703(2) 0.0216(10) Uani 1.00 1 d . . . C(108) C 0.5330(4) 0.2388(3) 0.6282(2) 0.0268(11) Uani 1.00 1 d . . . C(109) C 0.4251(5) 0.2363(4) 0.6237(2) 0.0336(13) Uani 1.00 1 d . . . C(110) C 0.3646(5) 0.2057(4) 0.6597(2) 0.0343(13) Uani 1.00 1 d . . . C(111) C 0.4126(5) 0.1779(4) 0.7013(2) 0.0349(13) Uani 1.00 1 d . . . C(112) C 0.5206(4) 0.1815(3) 0.7067(2) 0.0277(11) Uani 1.00 1 d . . . C(113) C 0.6420(4) 0.4378(3) 0.7144(2) 0.0218(10) Uani 1.00 1 d . . . C(114) C 0.6022(5) 0.4690(4) 0.6721(2) 0.0310(12) Uani 1.00 1 d . . . C(115) C 0.4968(6) 0.4764(5) 0.6663(3) 0.0454(16) Uani 1.00 1 d . . . C(116) C 0.4321(5) 0.4535(5) 0.7030(3) 0.0460(17) Uani 1.00 1 d . . . C(117) C 0.4714(5) 0.4229(4) 0.7450(3) 0.0431(16) Uani 1.00 1 d . . . C(118) C 0.5765(5) 0.4156(4) 0.7514(2) 0.0315(12) Uani 1.00 1 d . . . C(119) C 0.7321(4) 0.6503(3) 0.7881(2) 0.0252(11) Uani 1.00 1 d . . . C(120) C 0.7020(5) 0.6904(4) 0.7467(2) 0.0356(14) Uani 1.00 1 d . . . C(121) C 0.6035(6) 0.7116(5) 0.7426(3) 0.052(2) Uani 1.00 1 d . . . C(122) C 0.5359(6) 0.6941(6) 0.7785(3) 0.060(2) Uani 1.00 1 d . . . C(123) C 0.5628(6) 0.6545(5) 0.8184(3) 0.052(2) Uani 1.00 1 d . . . C(124) C 0.6622(5) 0.6329(4) 0.8238(2) 0.0364(14) Uani 1.00 1 d . . . C(125) C 0.8414(4) 0.8242(3) 0.8947(2) 0.0232(10) Uani 1.00 1 d . . . C(126) C 0.7983(4) 0.8694(3) 0.8603(2) 0.0261(11) Uani 1.00 1 d . . . C(127) C 0.7032(5) 0.8950(4) 0.8681(2) 0.0313(12) Uani 1.00 1 d . . . C(128) C 0.6518(5) 0.8788(4) 0.9108(2) 0.0346(13) Uani 1.00 1 d . . . C(129) C 0.6954(5) 0.8344(4) 0.9456(2) 0.0357(13) Uani 1.00 1 d . . . C(130) C 0.7898(4) 0.8078(3) 0.9378(2) 0.0285(11) Uani 1.00 1 d . . . C(131) C 1.0363(4) 0.8108(3) 0.9477(2) 0.0267(11) Uani 1.00 1 d . . . C(132) C 1.0585(5) 0.8999(4) 0.9774(2) 0.0422(16) Uani 1.00 1 d . . . C(133) C 1.1181(6) 0.9259(5) 1.0276(3) 0.0510(19) Uani 1.00 1 d . . . C(134) C 1.1594(6) 0.8649(5) 1.0487(3) 0.0516(19) Uani 1.00 1 d . . . C(135) C 1.1432(7) 0.7780(6) 1.0201(3) 0.060(2) Uani 1.00 1 d . . . C(136) C 1.0798(6) 0.7501(5) 0.9694(3) 0.0497(18) Uani 1.00 1 d . . . C(201) C 1.0449(4) 0.2408(3) 0.5537(2) 0.0197(9) Uani 1.00 1 d . . . C(202) C 0.9992(4) 0.2783(3) 0.5154(2) 0.0230(10) Uani 1.00 1 d . . . C(203) C 1.0465(4) 0.2849(3) 0.4697(2) 0.0281(11) Uani 1.00 1 d . . . C(204) C 1.1370(5) 0.2532(4) 0.4612(2) 0.0309(12) Uani 1.00 1 d . . . C(205) C 1.1821(5) 0.2135(4) 0.4985(2) 0.0315(12) Uani 1.00 1 d . . . C(206) C 1.1363(4) 0.2077(3) 0.5445(2) 0.0253(11) Uani 1.00 1 d . . . C(207) C 1.0188(4) 0.1424(3) 0.6334(2) 0.0204(9) Uani 1.00 1 d . . . C(208) C 1.0724(4) 0.1434(3) 0.6820(2) 0.0254(11) Uani 1.00 1 d . . . C(209) C 1.0930(5) 0.0643(4) 0.6932(2) 0.0354(13) Uani 1.00 1 d . . . C(210) C 1.0593(5) -0.0156(4) 0.6554(2) 0.0377(14) Uani 1.00 1 d . . . C(211) C 1.0059(6) -0.0177(4) 0.6060(3) 0.0422(15) Uani 1.00 1 d . . . C(212) C 0.9846(5) 0.0606(4) 0.5946(2) 0.0341(13) Uani 1.00 1 d . . . C(213) C 1.1179(4) 0.4651(3) 0.6034(2) 0.0191(9) Uani 1.00 1 d . . . C(214) C 1.0795(4) 0.5150(3) 0.5705(2) 0.0209(10) Uani 1.00 1 d . . . C(215) C 1.1347(4) 0.5354(3) 0.5295(2) 0.0264(11) Uani 1.00 1 d . . . C(216) C 1.2251(4) 0.5031(4) 0.5199(2) 0.0285(11) Uani 1.00 1 d . . . C(217) C 1.2628(4) 0.4526(3) 0.5522(2) 0.0274(11) Uani 1.00 1 d . . . C(218) C 1.2102(4) 0.4344(3) 0.5940(2) 0.0218(10) Uani 1.00 1 d . . . C(219) C 1.1965(4) 0.6800(3) 0.6772(2) 0.0194(9) Uani 1.00 1 d . . . C(220) C 1.1510(4) 0.7299(3) 0.6468(2) 0.0244(10) Uani 1.00 1 d . . . C(221) C 1.2063(5) 0.7644(4) 0.6094(2) 0.0312(12) Uani 1.00 1 d . . . C(222) C 1.3056(5) 0.7488(4) 0.6023(2) 0.0361(14) Uani 1.00 1 d . . . C(223) C 1.3512(5) 0.6989(4) 0.6321(2) 0.0326(12) Uani 1.00 1 d . . . C(224) C 1.2973(4) 0.6643(3) 0.6694(2) 0.0240(10) Uani 1.00 1 d . . . C(225) C 1.3079(4) 0.8658(3) 0.7838(2) 0.0240(10) Uani 1.00 1 d . . . C(226) C 1.2659(4) 0.9061(4) 0.7466(2) 0.0309(12) Uani 1.00 1 d . . . C(227) C 1.3311(5) 0.9506(4) 0.7169(2) 0.0383(14) Uani 1.00 1 d . . . C(228) C 1.4386(5) 0.9559(4) 0.7244(2) 0.0395(15) Uani 1.00 1 d . . . C(229) C 1.4814(5) 0.9174(4) 0.7619(2) 0.0373(14) Uani 1.00 1 d . . . C(230) C 1.4173(4) 0.8735(4) 0.7922(2) 0.0297(12) Uani 1.00 1 d . . . C(231) C 1.2963(4) 0.8238(4) 0.8852(2) 0.0300(12) Uani 1.00 1 d . . . C(232) C 1.3044(6) 0.9077(5) 0.9196(3) 0.053(2) Uani 1.00 1 d . . . C(233) C 1.3630(8) 0.9301(7) 0.9691(4) 0.079(3) Uani 1.00 1 d . . . C(234) C 1.4165(9) 0.8717(9) 0.9865(4) 0.084(3) Uani 1.00 1 d . . . C(235) C 1.4086(7) 0.7872(6) 0.9533(3) 0.060(2) Uani 1.00 1 d . . . C(236) C 1.3481(5) 0.7632(5) 0.9025(2) 0.0413(15) Uani 1.00 1 d . . . H(1) H 0.7261 0.3140 0.7628 0.024 Uiso 1.00 1 c R . . H(2) H 0.8417 0.3160 0.7516 0.024 Uiso 1.00 1 c R . . H(3) H 0.7814 0.4906 0.8117 0.021 Uiso 1.00 1 c R . . H(4) H 0.8957 0.4855 0.8005 0.021 Uiso 1.00 1 c R . . H(5) H 0.8651 0.6469 0.8839 0.027 Uiso 1.00 1 c R . . H(6) H 0.9762 0.6369 0.8692 0.027 Uiso 1.00 1 c R . . H(7) H 1.0541 0.3284 0.7010 0.022 Uiso 1.00 1 c R . . H(8) H 1.1407 0.3333 0.6635 0.022 Uiso 1.00 1 c R . . H(9) H 1.1134 0.5006 0.7481 0.022 Uiso 1.00 1 c R . . H(10) H 1.2026 0.5155 0.7129 0.022 Uiso 1.00 1 c R . . H(11) H 1.1957 0.6514 0.8149 0.021 Uiso 1.00 1 c R . . H(12) H 1.2848 0.6798 0.7820 0.021 Uiso 1.00 1 c R . . H(13) H 0.4985 0.0093 0.4469 0.076 Uiso 1.00 1 c R . . H(14) H 0.5558 0.0669 0.4121 0.076 Uiso 1.00 1 c R . . H(15) H 0.5585 -0.0336 0.4021 0.076 Uiso 1.00 1 c R . . H(16) H 0.7366 -0.0426 0.4898 0.152 Uiso 1.00 1 c R . . H(17) H 0.7010 -0.0652 0.4282 0.152 Uiso 1.00 1 c R . . H(18) H 0.7949 0.0140 0.4547 0.152 Uiso 1.00 1 c R . . H(19) H 1.0306 1.2365 0.8604 0.071 Uiso 1.00 1 c R . . H(20) H 1.0388 1.1803 0.8038 0.071 Uiso 1.00 1 c R . . H(21) H 0.9397 1.1564 0.8314 0.071 Uiso 1.00 1 c R . . H(22) H 1.0969 1.1256 0.9395 0.072 Uiso 1.00 1 c R . . H(23) H 1.1975 1.1487 0.9129 0.072 Uiso 1.00 1 c R . . H(24) H 1.1264 1.2177 0.9259 0.072 Uiso 1.00 1 c R . . H(25) H 0.6277 0.1503 0.5129 0.038 Uiso 1.00 1 c R . . H(26) H 1.0109 1.0129 0.8025 0.041 Uiso 1.00 1 c R . . H(27) H 0.7419 0.1747 0.7827 0.037 Uiso 1.00 1 c R . . H(28) H 0.7673 0.0455 0.8083 0.051 Uiso 1.00 1 c R . . H(29) H 0.7898 -0.0780 0.7443 0.052 Uiso 1.00 1 c R . . H(30) H 0.7876 -0.0723 0.6536 0.062 Uiso 1.00 1 c R . . H(31) H 0.7593 0.0560 0.6279 0.046 Uiso 1.00 1 c R . . H(32) H 0.5733 0.2596 0.6027 0.033 Uiso 1.00 1 c R . . H(33) H 0.3922 0.2563 0.5950 0.040 Uiso 1.00 1 c R . . H(34) H 0.2899 0.2024 0.6557 0.040 Uiso 1.00 1 c R . . H(35) H 0.3712 0.1570 0.7268 0.041 Uiso 1.00 1 c R . . H(36) H 0.5532 0.1628 0.7355 0.034 Uiso 1.00 1 c R . . H(37) H 0.6464 0.4841 0.6461 0.037 Uiso 1.00 1 c R . . H(38) H 0.4697 0.4983 0.6373 0.054 Uiso 1.00 1 c R . . H(39) H 0.3605 0.4592 0.6995 0.055 Uiso 1.00 1 c R . . H(40) H 0.4258 0.4061 0.7699 0.049 Uiso 1.00 1 c R . . H(41) H 0.6040 0.3948 0.7814 0.038 Uiso 1.00 1 c R . . H(42) H 0.7492 0.7016 0.7214 0.041 Uiso 1.00 1 c R . . H(43) H 0.5846 0.7410 0.7157 0.063 Uiso 1.00 1 c R . . H(44) H 0.4682 0.7087 0.7753 0.065 Uiso 1.00 1 c R . . H(45) H 0.5129 0.6412 0.8420 0.062 Uiso 1.00 1 c R . . H(46) H 0.6828 0.6061 0.8524 0.046 Uiso 1.00 1 c R . . H(47) H 0.8346 0.8820 0.8311 0.032 Uiso 1.00 1 c R . . H(48) H 0.6729 0.9249 0.8437 0.037 Uiso 1.00 1 c R . . H(49) H 0.5870 0.8975 0.9163 0.040 Uiso 1.00 1 c R . . H(50) H 0.6598 0.8238 0.9750 0.042 Uiso 1.00 1 c R . . H(51) H 0.8193 0.7773 0.9619 0.035 Uiso 1.00 1 c R . . H(52) H 1.0298 0.9431 0.9623 0.048 Uiso 1.00 1 c R . . H(53) H 1.1317 0.9874 1.0478 0.055 Uiso 1.00 1 c R . . H(54) H 1.1996 0.8825 1.0839 0.059 Uiso 1.00 1 c R . . H(55) H 1.1741 0.7345 1.0345 0.069 Uiso 1.00 1 c R . . H(56) H 1.0666 0.6889 0.9494 0.057 Uiso 1.00 1 c R . . H(57) H 0.9345 0.2988 0.5204 0.029 Uiso 1.00 1 c R . . H(58) H 1.0160 0.3124 0.4441 0.036 Uiso 1.00 1 c R . . H(59) H 1.1680 0.2572 0.4294 0.038 Uiso 1.00 1 c R . . H(60) H 1.2441 0.1905 0.4919 0.039 Uiso 1.00 1 c R . . H(61) H 1.1675 0.1806 0.5701 0.032 Uiso 1.00 1 c R . . H(62) H 1.0955 0.1988 0.7083 0.031 Uiso 1.00 1 c R . . H(63) H 1.1302 0.0665 0.7278 0.046 Uiso 1.00 1 c R . . H(64) H 1.0728 -0.0695 0.6630 0.050 Uiso 1.00 1 c R . . H(65) H 0.9824 -0.0736 0.5793 0.052 Uiso 1.00 1 c R . . H(66) H 0.9464 0.0592 0.5603 0.040 Uiso 1.00 1 c R . . H(67) H 1.0155 0.5350 0.5764 0.026 Uiso 1.00 1 c R . . H(68) H 1.1108 0.5723 0.5085 0.033 Uiso 1.00 1 c R . . H(69) H 1.2614 0.5158 0.4907 0.034 Uiso 1.00 1 c R . . H(70) H 1.3255 0.4308 0.5456 0.036 Uiso 1.00 1 c R . . H(71) H 1.2361 0.4001 0.6165 0.027 Uiso 1.00 1 c R . . H(72) H 1.0825 0.7410 0.6520 0.032 Uiso 1.00 1 c R . . H(73) H 1.1747 0.7983 0.5887 0.038 Uiso 1.00 1 c R . . H(74) H 1.3435 0.7724 0.5769 0.044 Uiso 1.00 1 c R . . H(75) H 1.4201 0.6886 0.6275 0.040 Uiso 1.00 1 c R . . H(76) H 1.3286 0.6289 0.6896 0.030 Uiso 1.00 1 c R . . H(77) H 1.1919 0.9034 0.7413 0.039 Uiso 1.00 1 c R . . H(78) H 1.2997 0.9774 0.6912 0.047 Uiso 1.00 1 c R . . H(79) H 1.4835 0.9872 0.7040 0.047 Uiso 1.00 1 c R . . H(80) H 1.5561 0.9193 0.7665 0.045 Uiso 1.00 1 c R . . H(81) H 1.4482 0.8508 0.8206 0.039 Uiso 1.00 1 c R . . H(82) H 1.2670 0.9494 0.9082 0.060 Uiso 1.00 1 c R . . H(83) H 1.3660 0.9879 0.9926 0.086 Uiso 1.00 1 c R . . H(84) H 1.4580 0.8867 1.0216 0.098 Uiso 1.00 1 c R . . H(85) H 1.4460 0.7455 0.9648 0.070 Uiso 1.00 1 c R . . H(86) H 1.3411 0.7043 0.8801 0.050 Uiso 1.00 1 c R . . H(87) H 0.4395 0.3888 0.3968 0.099 Uiso 1.00 1 c R . . H(88) H 0.4031 0.4287 0.4511 0.099 Uiso 1.00 1 c R . . H(89) H 0.3246 0.3560 0.4071 0.099 Uiso 1.00 1 c R . . H(90) H 0.4723 0.3586 0.5262 0.159 Uiso 1.00 1 c R . . H(91) H 0.5509 0.4024 0.4930 0.159 Uiso 1.00 1 c R . . H(92) H 0.5529 0.3072 0.5000 0.159 Uiso 1.00 1 c R . . H(93) H 0.4003 0.8642 0.1002 0.183 Uiso 1.00 1 c R . . H(94) H 0.4506 0.9270 0.1557 0.183 Uiso 1.00 1 c R . . H(95) H 0.3640 0.8428 0.1525 0.183 Uiso 1.00 1 c R . . H(96) H 0.6414 0.8916 0.1779 0.160 Uiso 1.00 1 c R . . H(97) H 0.6090 0.9131 0.1235 0.160 Uiso 1.00 1 c R . . H(98) H 0.6512 0.8272 0.1242 0.160 Uiso 1.00 1 c R . . H(99) H 0.3540 0.5272 0.0063 0.146 Uiso 0.50 1 c R . . H(100) H 0.2997 0.5702 -0.0344 0.146 Uiso 0.50 1 c R . . H(101) H 0.3740 0.6304 0.0162 0.146 Uiso 0.50 1 c R . . H(102) H 0.4393 0.5187 -0.1257 0.189 Uiso 0.50 1 c R . . H(103) H 0.3846 0.4552 -0.0932 0.189 Uiso 0.50 1 c R . . H(104) H 0.5057 0.4689 -0.0943 0.189 Uiso 0.50 1 c R . . H(105) H 0.2070 0.4305 -0.0374 0.127 Uiso 0.50 1 c R . . H(106) H 0.1075 0.3630 -0.0318 0.127 Uiso 0.50 1 c R . . H(107) H 0.2101 0.3810 0.0084 0.127 Uiso 0.50 1 c R . . H(108) H -0.0216 0.5058 0.0326 0.133 Uiso 0.50 1 c R . . H(109) H 0.0157 0.5212 -0.0208 0.133 Uiso 0.50 1 c R . . H(110) H 0.0572 0.5931 0.0327 0.133 Uiso 0.50 1 c R . . H(111) H 0.3552 0.1750 0.4001 0.146 Uiso 1.00 1 c R . . H(112) H 0.5229 0.6954 0.1551 0.146 Uiso 1.00 1 c R . . H(113) H 0.6291 0.6003 -0.0427 0.120 Uiso 0.50 1 c R . . H(114) H 0.1811 0.5941 0.0971 0.120 Uiso 0.50 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0194(3) 0.0194(3) 0.0196(3) 0.0044(2) 0.0032(2) 0.0044(2) Cu(2) 0.0177(3) 0.0184(2) 0.0186(3) 0.0042(2) 0.0034(2) 0.0056(2) Cu(3) 0.0174(3) 0.0183(2) 0.0191(3) 0.0045(2) 0.0038(2) 0.0047(2) Cu(4) 0.0219(3) 0.0224(3) 0.0242(3) 0.0047(2) 0.0070(2) 0.0035(2) Cu(5) 0.0489(5) 0.0522(5) 0.0493(5) 0.0114(4) 0.0109(4) 0.0207(4) Cl(1) 0.0221(6) 0.0212(5) 0.0209(5) 0.0052(4) -0.0000(4) 0.0053(4) Cl(2) 0.0214(6) 0.0205(5) 0.0211(5) 0.0056(4) 0.0008(4) 0.0054(4) Cl(3) 0.0242(6) 0.0221(5) 0.0256(6) 0.0061(4) 0.0020(4) 0.0055(4) Cl(11) 0.0768(15) 0.0751(14) 0.0739(14) 0.0514(12) 0.0322(12) 0.0457(12) Cl(12) 0.0685(15) 0.0736(15) 0.0770(16) -0.0016(12) 0.0261(13) -0.0098(12) P(1) 0.0176(6) 0.0165(5) 0.0185(5) 0.0024(4) 0.0039(4) 0.0047(4) P(2) 0.0153(6) 0.0150(5) 0.0162(5) 0.0017(4) 0.0033(4) 0.0027(4) P(3) 0.0156(6) 0.0159(5) 0.0168(5) 0.0030(4) 0.0033(4) 0.0008(4) P(4) 0.0199(6) 0.0196(6) 0.0204(6) 0.0030(4) 0.0046(5) -0.0011(4) P(5) 0.0173(6) 0.0159(5) 0.0173(5) 0.0048(4) 0.0028(4) 0.0039(4) P(6) 0.0152(5) 0.0146(5) 0.0153(5) 0.0036(4) 0.0034(4) 0.0032(4) P(7) 0.0142(5) 0.0143(5) 0.0153(5) 0.0021(4) 0.0030(4) 0.0025(4) P(8) 0.0178(6) 0.0187(6) 0.0195(6) 0.0009(4) 0.0026(4) -0.0009(4) O(1) 0.044(2) 0.038(2) 0.041(2) 0.012(2) -0.011(2) -0.008(2) O(2) 0.042(2) 0.036(2) 0.041(2) 0.006(2) 0.000(2) -0.002(2) O(11) 0.105(7) 0.118(8) 0.120(8) 0.012(6) 0.010(6) 0.020(6) O(12) 0.132(10) 0.138(10) 0.133(10) -0.008(8) 0.009(8) -0.005(7) O(13) 0.058(7) 0.056(7) 0.056(7) -0.002(5) -0.001(5) 0.006(5) O(14) 0.094(12) 0.093(12) 0.081(11) 0.008(9) 0.007(9) 0.006(9) N(1) 0.045(3) 0.041(3) 0.041(3) 0.011(2) -0.013(2) -0.011(2) N(2) 0.038(3) 0.033(2) 0.041(3) 0.003(2) 0.012(2) 0.005(2) N(11) 0.049(4) 0.055(4) 0.057(4) 0.005(3) 0.008(3) 0.008(3) N(12) 0.089(7) 0.083(7) 0.081(6) 0.007(5) 0.003(5) 0.010(5) N(13) 0.079(12) 0.074(11) 0.077(12) -0.000(9) 0.003(9) 0.012(9) N(14) 0.083(13) 0.085(13) 0.090(14) 0.008(11) 0.008(11) 0.016(11) C(1) 0.019(2) 0.019(2) 0.021(2) 0.0014(18) 0.0036(19) 0.0063(18) C(2) 0.017(2) 0.017(2) 0.017(2) -0.0013(17) -0.0009(18) -0.0005(17) C(3) 0.021(2) 0.020(2) 0.021(2) 0.0030(19) 0.0032(19) -0.0008(19) C(4) 0.019(2) 0.018(2) 0.017(2) 0.0058(18) 0.0049(18) 0.0073(17) C(5) 0.018(2) 0.017(2) 0.017(2) 0.0051(18) 0.0027(18) 0.0037(17) C(6) 0.017(2) 0.017(2) 0.017(2) -0.0003(17) 0.0021(18) 0.0033(17) C(11) 0.033(3) 0.029(2) 0.030(3) 0.006(2) 0.003(2) 0.001(2) C(12) 0.059(5) 0.059(5) 0.061(5) 0.006(4) -0.026(4) -0.007(4) C(13) 0.129(12) 0.126(12) 0.132(12) 0.080(10) -0.071(10) -0.087(10) C(21) 0.034(3) 0.032(3) 0.035(3) -0.000(2) 0.007(2) 0.000(2) C(22) 0.059(5) 0.050(4) 0.064(5) 0.010(3) 0.016(4) 0.024(3) C(23) 0.057(5) 0.054(5) 0.061(5) 0.004(4) 0.001(4) -0.017(4) C(31) 0.106(13) 0.19(2) 0.140(17) -0.007(13) 0.027(12) -0.013(15) C(32) 0.084(8) 0.094(8) 0.084(8) 0.016(6) 0.010(6) 0.014(6) C(33) 0.121(14) 0.169(18) 0.123(14) 0.027(12) 0.009(11) 0.003(12) C(34) 0.16(2) 0.16(2) 0.18(2) -0.014(16) -0.013(17) 0.028(17) C(35) 0.158(19) 0.19(2) 0.120(15) 0.039(16) 0.006(13) 0.016(14) C(36) 0.125(14) 0.133(15) 0.137(15) 0.003(11) 0.017(11) -0.002(11) C(37) 0.067(12) 0.071(13) 0.073(13) 0.001(10) 0.004(10) 0.015(10) C(38) 0.10(2) 0.10(2) 0.12(2) 0.008(16) 0.008(18) 0.018(17) C(39) 0.11(2) 0.081(16) 0.074(15) -0.020(14) -0.002(13) -0.001(12) C(40) 0.073(14) 0.078(14) 0.066(13) 0.000(11) 0.005(11) 0.012(10) C(41) 0.12(2) 0.093(19) 0.094(19) -0.001(17) 0.006(17) 0.001(15) C(42) 0.13(3) 0.12(2) 0.13(2) 0.01(2) 0.02(2) 0.03(2) C(101) 0.023(2) 0.022(2) 0.025(2) 0.002(2) 0.004(2) 0.008(2) C(102) 0.034(3) 0.030(2) 0.032(3) 0.006(2) 0.003(2) 0.012(2) C(103) 0.041(3) 0.040(3) 0.043(3) 0.007(2) 0.001(2) 0.027(3) C(104) 0.040(3) 0.038(3) 0.049(3) 0.009(2) 0.006(3) 0.027(3) C(105) 0.052(4) 0.043(3) 0.056(4) 0.019(3) 0.024(3) 0.018(3) C(106) 0.043(3) 0.033(3) 0.039(3) 0.012(2) 0.017(2) 0.010(2) C(107) 0.021(2) 0.019(2) 0.022(2) -0.0001(19) 0.003(2) 0.0009(19) C(108) 0.026(2) 0.026(2) 0.027(2) 0.004(2) 0.001(2) 0.004(2) C(109) 0.031(3) 0.032(3) 0.033(3) 0.005(2) -0.005(2) 0.003(2) C(110) 0.029(3) 0.033(3) 0.037(3) 0.004(2) 0.004(2) 0.003(2) C(111) 0.032(3) 0.034(3) 0.037(3) -0.002(2) 0.013(2) 0.007(2) C(112) 0.026(2) 0.026(2) 0.029(2) 0.000(2) 0.005(2) 0.008(2) C(113) 0.020(2) 0.020(2) 0.023(2) 0.0024(19) 0.002(2) 0.0019(19) C(114) 0.028(3) 0.029(2) 0.033(3) 0.004(2) -0.004(2) 0.009(2) C(115) 0.040(4) 0.043(3) 0.050(4) 0.008(3) -0.012(3) 0.013(3) C(116) 0.036(3) 0.041(3) 0.052(4) 0.005(3) 0.001(3) -0.004(3) C(117) 0.035(3) 0.041(3) 0.045(3) 0.003(2) 0.012(3) -0.007(2) C(118) 0.029(3) 0.031(2) 0.032(3) 0.004(2) 0.011(2) 0.001(2) C(119) 0.022(2) 0.023(2) 0.025(2) 0.003(2) 0.003(2) -0.005(2) C(120) 0.033(3) 0.035(3) 0.034(3) 0.018(2) -0.006(2) -0.006(2) C(121) 0.047(4) 0.051(4) 0.049(4) 0.025(3) -0.013(3) -0.014(3) C(122) 0.044(4) 0.054(4) 0.064(5) 0.016(3) -0.008(4) -0.022(4) C(123) 0.043(4) 0.046(4) 0.057(4) 0.001(3) 0.021(3) -0.009(3) C(124) 0.033(3) 0.035(3) 0.041(3) 0.006(2) 0.019(2) 0.003(2) C(125) 0.022(2) 0.021(2) 0.021(2) 0.0021(19) 0.004(2) -0.0029(19) C(126) 0.025(2) 0.025(2) 0.025(2) 0.003(2) 0.003(2) 0.001(2) C(127) 0.029(3) 0.029(2) 0.031(3) 0.005(2) -0.000(2) -0.002(2) C(128) 0.029(3) 0.033(3) 0.033(3) 0.004(2) 0.000(2) -0.009(2) C(129) 0.034(3) 0.036(3) 0.034(3) 0.007(2) 0.013(2) -0.002(2) C(130) 0.029(3) 0.029(2) 0.028(2) 0.008(2) 0.010(2) 0.003(2) C(131) 0.023(2) 0.026(2) 0.024(2) 0.001(2) 0.001(2) -0.004(2) C(132) 0.037(3) 0.036(3) 0.039(3) 0.003(2) -0.009(2) -0.010(2) C(133) 0.043(4) 0.047(4) 0.044(4) 0.003(3) -0.005(3) -0.018(3) C(134) 0.045(4) 0.053(4) 0.042(4) 0.004(3) -0.009(3) -0.009(3) C(135) 0.059(5) 0.058(5) 0.053(4) 0.014(4) -0.022(4) 0.004(3) C(136) 0.051(4) 0.044(4) 0.044(4) 0.014(3) -0.013(3) -0.006(3) C(201) 0.020(2) 0.019(2) 0.018(2) 0.0046(18) 0.0021(19) 0.0007(18) C(202) 0.024(2) 0.023(2) 0.024(2) 0.009(2) 0.003(2) 0.006(2) C(203) 0.030(3) 0.028(2) 0.027(2) 0.006(2) 0.004(2) 0.007(2) C(204) 0.033(3) 0.031(2) 0.030(2) 0.007(2) 0.013(2) 0.006(2) C(205) 0.032(3) 0.035(3) 0.033(3) 0.020(2) 0.013(2) 0.007(2) C(206) 0.027(2) 0.026(2) 0.025(2) 0.012(2) 0.004(2) 0.005(2) C(207) 0.021(2) 0.020(2) 0.022(2) 0.0055(19) 0.0052(19) 0.0078(19) C(208) 0.027(2) 0.026(2) 0.026(2) 0.009(2) 0.004(2) 0.009(2) C(209) 0.040(3) 0.037(3) 0.039(3) 0.017(2) 0.007(2) 0.021(2) C(210) 0.041(3) 0.038(3) 0.046(3) 0.014(2) 0.011(2) 0.028(3) C(211) 0.043(4) 0.036(3) 0.046(3) 0.008(2) 0.001(3) 0.010(2) C(212) 0.035(3) 0.029(3) 0.036(3) 0.007(2) -0.003(2) 0.008(2) C(213) 0.020(2) 0.017(2) 0.018(2) 0.0042(18) 0.0029(19) 0.0003(18) C(214) 0.023(2) 0.021(2) 0.022(2) 0.0086(19) 0.008(2) 0.0069(19) C(215) 0.030(2) 0.027(2) 0.027(2) 0.009(2) 0.009(2) 0.010(2) C(216) 0.031(3) 0.029(2) 0.029(2) 0.007(2) 0.013(2) 0.010(2) C(217) 0.029(3) 0.030(2) 0.029(2) 0.012(2) 0.015(2) 0.012(2) C(218) 0.022(2) 0.023(2) 0.022(2) 0.007(2) 0.005(2) 0.008(2) C(219) 0.019(2) 0.018(2) 0.020(2) -0.0004(18) 0.0032(19) 0.0040(18) C(220) 0.026(2) 0.025(2) 0.025(2) 0.006(2) 0.005(2) 0.008(2) C(221) 0.033(3) 0.030(2) 0.030(2) 0.001(2) 0.003(2) 0.011(2) C(222) 0.037(3) 0.036(3) 0.036(3) -0.002(2) 0.019(2) 0.013(2) C(223) 0.030(3) 0.034(3) 0.034(3) 0.003(2) 0.012(2) 0.009(2) C(224) 0.022(2) 0.025(2) 0.024(2) 0.003(2) 0.005(2) 0.006(2) C(225) 0.023(2) 0.021(2) 0.025(2) 0.003(2) 0.004(2) 0.002(2) C(226) 0.028(3) 0.030(2) 0.033(3) 0.000(2) 0.001(2) 0.010(2) C(227) 0.038(3) 0.038(3) 0.040(3) -0.001(2) -0.001(2) 0.022(2) C(228) 0.038(3) 0.039(3) 0.042(3) -0.005(2) 0.009(2) 0.021(2) C(229) 0.032(3) 0.038(3) 0.040(3) -0.004(2) 0.004(2) 0.017(2) C(230) 0.028(3) 0.031(2) 0.032(3) 0.004(2) 0.006(2) 0.012(2) C(231) 0.025(2) 0.031(2) 0.026(2) -0.001(2) 0.001(2) -0.004(2) C(232) 0.043(4) 0.050(4) 0.046(4) 0.002(3) -0.004(3) -0.021(3) C(233) 0.060(6) 0.079(7) 0.063(6) -0.004(5) -0.005(4) -0.037(5) C(234) 0.065(6) 0.098(8) 0.060(6) -0.006(6) -0.007(5) -0.015(5) C(235) 0.052(4) 0.071(5) 0.055(5) -0.002(4) -0.008(3) 0.029(4) C(236) 0.039(3) 0.044(3) 0.038(3) 0.003(2) -0.003(2) 0.011(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) Cl(1) 2.3220(15) yes . . Cu(1) P(1) 2.2262(15) yes . . Cu(1) P(5) 2.2477(14) yes . . Cu(1) O(1) 2.155(4) yes . . Cu(2) Cl(1) 2.4288(11) yes . . Cu(2) Cl(2) 2.4020(15) yes . . Cu(2) P(2) 2.2601(14) yes . . Cu(2) P(6) 2.2575(14) yes . . Cu(3) Cl(2) 2.3817(12) yes . . Cu(3) Cl(3) 2.4569(14) yes . . Cu(3) P(3) 2.2413(14) yes . . Cu(3) P(7) 2.2366(15) yes . . Cu(4) Cl(3) 2.3171(14) yes . . Cu(4) P(4) 2.2299(16) yes . . Cu(4) P(8) 2.2338(16) yes . . Cu(4) O(2) 2.189(4) yes . . Cu(5) Cl(11) 2.085(2) yes . . Cu(5) Cl(12) 2.085(3) yes . . P(1) C(1) 1.843(4) yes . . P(1) C(101) 1.824(6) yes . . P(1) C(107) 1.828(5) yes . . P(2) C(1) 1.845(5) yes . . P(2) C(2) 1.840(4) yes . . P(2) C(113) 1.823(5) yes . . P(3) C(2) 1.848(5) yes . . P(3) C(3) 1.843(5) yes . . P(3) C(119) 1.819(6) yes . . P(4) C(3) 1.835(5) yes . . P(4) C(125) 1.828(6) yes . . P(4) C(131) 1.807(5) yes . . P(5) C(4) 1.851(4) yes . . P(5) C(201) 1.827(5) yes . . P(5) C(207) 1.827(6) yes . . P(6) C(4) 1.849(5) yes . . P(6) C(5) 1.847(4) yes . . P(6) C(213) 1.822(5) yes . . P(7) C(5) 1.850(5) yes . . P(7) C(6) 1.844(4) yes . . P(7) C(219) 1.824(5) yes . . P(8) C(6) 1.841(5) yes . . P(8) C(225) 1.829(6) yes . . P(8) C(231) 1.825(6) yes . . O(1) C(11) 1.231(7) yes . . O(2) C(21) 1.237(9) yes . . O(11) C(31) 1.31(2) yes . . O(12) C(34) 1.35(2) yes . . O(13) C(37) 1.28(2) yes . . O(14) C(40) 1.27(3) yes . . N(1) C(11) 1.319(7) yes . . N(1) C(12) 1.456(11) yes . . N(1) C(13) 1.435(19) yes . . N(2) C(21) 1.324(8) yes . . N(2) C(22) 1.453(12) yes . . N(2) C(23) 1.425(10) yes . . N(11) C(31) 1.55(2) yes . . N(11) C(32) 1.393(18) yes . . N(11) C(33) 1.495(19) yes . . N(12) C(34) 1.36(3) yes . . N(12) C(35) 1.40(3) yes . . N(12) C(36) 1.43(2) yes . . N(13) C(37) 1.42(2) yes . . N(13) C(38) 1.63(4) yes . . N(13) C(39) 1.59(3) yes . . N(14) C(40) 1.29(2) yes . . N(14) C(41) 1.54(3) yes . . N(14) C(42) 1.45(4) yes . . C(101) C(102) 1.387(8) yes . . C(101) C(106) 1.400(8) yes . . C(102) C(103) 1.398(10) yes . . C(103) C(104) 1.373(9) yes . . C(104) C(105) 1.384(12) yes . . C(105) C(106) 1.384(11) yes . . C(107) C(108) 1.387(8) yes . . C(107) C(112) 1.395(8) yes . . C(108) C(109) 1.388(9) yes . . C(109) C(110) 1.376(10) yes . . C(110) C(111) 1.383(10) yes . . C(111) C(112) 1.386(9) yes . . C(113) C(114) 1.385(9) yes . . C(113) C(118) 1.392(9) yes . . C(114) C(115) 1.393(10) yes . . C(115) C(116) 1.383(12) yes . . C(116) C(117) 1.372(12) yes . . C(117) C(118) 1.389(10) yes . . C(119) C(120) 1.413(9) yes . . C(119) C(124) 1.385(9) yes . . C(120) C(121) 1.382(11) yes . . C(121) C(122) 1.368(13) yes . . C(122) C(123) 1.364(14) yes . . C(123) C(124) 1.398(11) yes . . C(125) C(126) 1.391(9) yes . . C(125) C(130) 1.394(8) yes . . C(126) C(127) 1.388(9) yes . . C(127) C(128) 1.382(9) yes . . C(128) C(129) 1.393(10) yes . . C(129) C(130) 1.386(9) yes . . C(131) C(132) 1.399(8) yes . . C(131) C(136) 1.385(11) yes . . C(132) C(133) 1.380(10) yes . . C(133) C(134) 1.367(13) yes . . C(134) C(135) 1.368(11) yes . . C(135) C(136) 1.411(11) yes . . C(201) C(202) 1.396(8) yes . . C(201) C(206) 1.402(8) yes . . C(202) C(203) 1.391(8) yes . . C(203) C(204) 1.376(9) yes . . C(204) C(205) 1.397(10) yes . . C(205) C(206) 1.386(9) yes . . C(207) C(208) 1.370(8) yes . . C(207) C(212) 1.410(7) yes . . C(208) C(209) 1.402(10) yes . . C(209) C(210) 1.375(8) yes . . C(210) C(211) 1.381(10) yes . . C(211) C(212) 1.397(11) yes . . C(213) C(214) 1.393(8) yes . . C(213) C(218) 1.394(8) yes . . C(214) C(215) 1.389(8) yes . . C(215) C(216) 1.383(9) yes . . C(216) C(217) 1.386(9) yes . . C(217) C(218) 1.381(8) yes . . C(219) C(220) 1.391(8) yes . . C(219) C(224) 1.400(8) yes . . C(220) C(221) 1.394(9) yes . . C(221) C(222) 1.379(10) yes . . C(222) C(223) 1.382(10) yes . . C(223) C(224) 1.387(9) yes . . C(225) C(226) 1.384(9) yes . . C(225) C(230) 1.396(8) yes . . C(226) C(227) 1.386(10) yes . . C(227) C(228) 1.376(10) yes . . C(228) C(229) 1.375(11) yes . . C(229) C(230) 1.387(10) yes . . C(231) C(232) 1.395(9) yes . . C(231) C(236) 1.390(11) yes . . C(232) C(233) 1.361(13) yes . . C(233) C(234) 1.373(19) yes . . C(234) C(235) 1.390(15) yes . . C(235) C(236) 1.398(11) yes . . C(1) H(1) 0.949 no . . C(1) H(2) 0.950 no . . C(2) H(3) 0.949 no . . C(2) H(4) 0.946 no . . C(3) H(5) 0.960 no . . C(3) H(6) 0.947 no . . C(4) H(7) 0.949 no . . C(4) H(8) 0.956 no . . C(5) H(9) 0.955 no . . C(5) H(10) 0.954 no . . C(6) H(11) 0.949 no . . C(6) H(12) 0.953 no . . C(11) H(25) 0.954 no . . C(12) H(13) 0.959 no . . C(12) H(14) 0.953 no . . C(12) H(15) 0.950 no . . C(13) H(16) 0.969 no . . C(13) H(17) 0.948 no . . C(13) H(18) 0.949 no . . C(21) H(26) 0.965 no . . C(22) H(19) 0.951 no . . C(22) H(20) 0.956 no . . C(22) H(21) 0.947 no . . C(23) H(22) 0.972 no . . C(23) H(23) 0.951 no . . C(23) H(24) 0.950 no . . C(31) H(111) 1.052 no . . C(32) H(87) 0.945 no . . C(32) H(88) 0.939 no . . C(32) H(89) 0.993 no . . C(33) H(90) 0.948 no . . C(33) H(91) 0.933 no . . C(33) H(92) 1.005 no . . C(34) H(112) 0.987 no . . C(35) H(93) 0.887 no . . C(35) H(94) 1.017 no . . C(35) H(95) 0.967 no . . C(36) H(96) 0.946 no . . C(36) H(97) 0.974 no . . C(36) H(98) 0.959 no . . C(37) H(113) 1.077 no . . C(38) H(99) 1.064 no . . C(38) H(100) 1.129 no . . C(38) H(101) 0.761 no . . C(39) H(102) 0.985 no . . C(39) H(103) 1.070 no . . C(39) H(104) 0.784 no . . C(40) H(114) 1.143 no . . C(41) H(105) 1.179 no . . C(41) H(106) 0.983 no . . C(41) H(107) 0.932 no . . C(42) H(108) 0.946 no . . C(42) H(109) 1.050 no . . C(42) H(110) 0.950 no . . C(102) H(27) 0.956 no . . C(103) H(28) 0.962 no . . C(104) H(29) 0.956 no . . C(105) H(30) 0.958 no . . C(106) H(31) 0.955 no . . C(108) H(32) 0.953 no . . C(109) H(33) 0.960 no . . C(110) H(34) 0.957 no . . C(111) H(35) 0.959 no . . C(112) H(36) 0.950 no . . C(114) H(37) 0.960 no . . C(115) H(38) 0.953 no . . C(116) H(39) 0.949 no . . C(117) H(40) 0.957 no . . C(118) H(41) 0.967 no . . C(120) H(42) 0.955 no . . C(121) H(43) 0.954 no . . C(122) H(44) 0.950 no . . C(123) H(45) 0.954 no . . C(124) H(46) 0.965 no . . C(126) H(47) 0.960 no . . C(127) H(48) 0.963 no . . C(128) H(49) 0.954 no . . C(129) H(50) 0.951 no . . C(130) H(51) 0.959 no . . C(132) H(52) 0.968 no . . C(133) H(53) 0.966 no . . C(134) H(54) 0.958 no . . C(135) H(55) 0.977 no . . C(136) H(56) 0.959 no . . C(202) H(57) 0.964 no . . C(203) H(58) 0.959 no . . C(204) H(59) 0.955 no . . C(205) H(60) 0.956 no . . C(206) H(61) 0.959 no . . C(208) H(62) 0.954 no . . C(209) H(63) 0.963 no . . C(210) H(64) 0.954 no . . C(211) H(65) 0.963 no . . C(212) H(66) 0.966 no . . C(214) H(67) 0.955 no . . C(215) H(68) 0.950 no . . C(216) H(69) 0.962 no . . C(217) H(70) 0.955 no . . C(218) H(71) 0.954 no . . C(220) H(72) 0.953 no . . C(221) H(73) 0.951 no . . C(222) H(74) 0.951 no . . C(223) H(75) 0.952 no . . C(224) H(76) 0.958 no . . C(226) H(77) 0.950 no . . C(227) H(78) 0.958 no . . C(228) H(79) 0.958 no . . C(229) H(80) 0.961 no . . C(230) H(81) 0.967 no . . C(232) H(82) 0.964 no . . C(233) H(83) 0.965 no . . C(234) H(84) 0.968 no . . C(235) H(85) 0.965 no . . C(236) H(86) 0.958 no . . H(108) H(109) 0.488 no . 2_565 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Cu(1) P(1) 113.04(5) yes . . . Cl(1) Cu(1) P(5) 115.24(5) yes . . . Cl(1) Cu(1) O(1) 101.46(15) yes . . . P(1) Cu(1) P(5) 118.42(5) yes . . . P(1) Cu(1) O(1) 108.45(15) yes . . . P(5) Cu(1) O(1) 97.04(15) yes . . . Cl(1) Cu(2) Cl(2) 101.90(4) yes . . . Cl(1) Cu(2) P(2) 104.95(4) yes . . . Cl(1) Cu(2) P(6) 111.88(4) yes . . . Cl(2) Cu(2) P(2) 107.92(5) yes . . . Cl(2) Cu(2) P(6) 108.29(5) yes . . . P(2) Cu(2) P(6) 120.31(5) yes . . . Cl(2) Cu(3) Cl(3) 101.04(4) yes . . . Cl(2) Cu(3) P(3) 108.89(4) yes . . . Cl(2) Cu(3) P(7) 107.53(4) yes . . . Cl(3) Cu(3) P(3) 107.37(5) yes . . . Cl(3) Cu(3) P(7) 109.32(4) yes . . . P(3) Cu(3) P(7) 120.90(5) yes . . . Cl(3) Cu(4) P(4) 116.13(5) yes . . . Cl(3) Cu(4) P(8) 114.95(5) yes . . . Cl(3) Cu(4) O(2) 102.11(14) yes . . . P(4) Cu(4) P(8) 116.19(6) yes . . . P(4) Cu(4) O(2) 101.61(14) yes . . . P(8) Cu(4) O(2) 102.46(14) yes . . . Cl(11) Cu(5) Cl(12) 178.86(12) yes . . . Cu(1) Cl(1) Cu(2) 83.12(4) yes . . . Cu(2) Cl(2) Cu(3) 89.07(5) yes . . . Cu(3) Cl(3) Cu(4) 81.85(4) yes . . . Cu(1) P(1) C(1) 110.87(18) yes . . . Cu(1) P(1) C(101) 114.57(19) yes . . . Cu(1) P(1) C(107) 119.39(18) yes . . . C(1) P(1) C(101) 103.4(2) yes . . . C(1) P(1) C(107) 103.6(2) yes . . . C(101) P(1) C(107) 103.3(2) yes . . . Cu(2) P(2) C(1) 116.81(18) yes . . . Cu(2) P(2) C(2) 116.11(17) yes . . . Cu(2) P(2) C(113) 117.5(2) yes . . . C(1) P(2) C(2) 98.8(2) yes . . . C(1) P(2) C(113) 102.6(2) yes . . . C(2) P(2) C(113) 102.3(2) yes . . . Cu(3) P(3) C(2) 116.26(17) yes . . . Cu(3) P(3) C(3) 117.61(18) yes . . . Cu(3) P(3) C(119) 114.4(2) yes . . . C(2) P(3) C(3) 98.3(2) yes . . . C(2) P(3) C(119) 103.8(2) yes . . . C(3) P(3) C(119) 104.2(2) yes . . . Cu(4) P(4) C(3) 111.91(18) yes . . . Cu(4) P(4) C(125) 119.8(2) yes . . . Cu(4) P(4) C(131) 113.47(19) yes . . . C(3) P(4) C(125) 102.9(2) yes . . . C(3) P(4) C(131) 104.8(2) yes . . . C(125) P(4) C(131) 102.3(2) yes . . . Cu(1) P(5) C(4) 112.86(18) yes . . . Cu(1) P(5) C(201) 116.25(18) yes . . . Cu(1) P(5) C(207) 116.24(17) yes . . . C(4) P(5) C(201) 104.7(2) yes . . . C(4) P(5) C(207) 103.3(2) yes . . . C(201) P(5) C(207) 101.9(2) yes . . . Cu(2) P(6) C(4) 114.46(16) yes . . . Cu(2) P(6) C(5) 114.31(17) yes . . . Cu(2) P(6) C(213) 119.74(18) yes . . . C(4) P(6) C(5) 100.3(2) yes . . . C(4) P(6) C(213) 104.2(2) yes . . . C(5) P(6) C(213) 101.2(2) yes . . . Cu(3) P(7) C(5) 114.84(16) yes . . . Cu(3) P(7) C(6) 115.81(17) yes . . . Cu(3) P(7) C(219) 116.95(19) yes . . . C(5) P(7) C(6) 98.6(2) yes . . . C(5) P(7) C(219) 105.6(2) yes . . . C(6) P(7) C(219) 102.7(2) yes . . . Cu(4) P(8) C(6) 113.84(16) yes . . . Cu(4) P(8) C(225) 116.4(2) yes . . . Cu(4) P(8) C(231) 115.0(2) yes . . . C(6) P(8) C(225) 105.0(2) yes . . . C(6) P(8) C(231) 102.9(2) yes . . . C(225) P(8) C(231) 102.1(2) yes . . . Cu(1) O(1) C(11) 129.5(4) yes . . . Cu(4) O(2) C(21) 124.5(3) yes . . . C(11) N(1) C(12) 123.1(7) yes . . . C(11) N(1) C(13) 120.2(7) yes . . . C(12) N(1) C(13) 116.6(8) yes . . . C(21) N(2) C(22) 120.9(5) yes . . . C(21) N(2) C(23) 121.5(7) yes . . . C(22) N(2) C(23) 117.6(6) yes . . . C(31) N(11) C(32) 142.4(9) yes . . . C(31) N(11) C(33) 108.9(13) yes . . . C(32) N(11) C(33) 108.6(11) yes . . . C(34) N(12) C(35) 116.3(16) yes . . . C(34) N(12) C(36) 125.7(16) yes . . . C(35) N(12) C(36) 117.5(16) yes . . . C(37) N(13) C(38) 116.3(17) yes . . . C(37) N(13) C(39) 115.4(19) yes . . . C(38) N(13) C(39) 126.5(18) yes . . . C(40) N(14) C(41) 114(2) yes . . . C(40) N(14) C(42) 120(2) yes . . . C(41) N(14) C(42) 126(2) yes . . . P(1) C(1) P(2) 113.0(2) yes . . . P(2) C(2) P(3) 114.2(2) yes . . . P(3) C(3) P(4) 111.9(3) yes . . . P(5) C(4) P(6) 111.8(2) yes . . . P(6) C(5) P(7) 114.6(2) yes . . . P(7) C(6) P(8) 113.2(2) yes . . . O(1) C(11) N(1) 123.7(6) yes . . . O(2) C(21) N(2) 124.4(6) yes . . . O(11) C(31) N(11) 101.9(12) yes . . . O(12) C(34) N(12) 114(2) yes . . . O(13) C(37) N(13) 124.1(19) yes . . . O(14) C(40) N(14) 124(2) yes . . . P(1) C(101) C(102) 124.6(4) yes . . . P(1) C(101) C(106) 117.2(4) yes . . . C(102) C(101) C(106) 118.2(6) yes . . . C(101) C(102) C(103) 120.4(5) yes . . . C(102) C(103) C(104) 120.5(7) yes . . . C(103) C(104) C(105) 119.9(7) yes . . . C(104) C(105) C(106) 119.9(7) yes . . . C(101) C(106) C(105) 121.1(6) yes . . . P(1) C(107) C(108) 118.7(4) yes . . . P(1) C(107) C(112) 122.7(4) yes . . . C(108) C(107) C(112) 118.6(5) yes . . . C(107) C(108) C(109) 120.1(5) yes . . . C(108) C(109) C(110) 121.1(6) yes . . . C(109) C(110) C(111) 119.3(6) yes . . . C(110) C(111) C(112) 120.0(6) yes . . . C(107) C(112) C(111) 120.9(6) yes . . . P(2) C(113) C(114) 119.1(4) yes . . . P(2) C(113) C(118) 121.3(4) yes . . . C(114) C(113) C(118) 119.6(5) yes . . . C(113) C(114) C(115) 119.9(6) yes . . . C(114) C(115) C(116) 120.1(7) yes . . . C(115) C(116) C(117) 120.0(7) yes . . . C(116) C(117) C(118) 120.4(7) yes . . . C(113) C(118) C(117) 119.9(6) yes . . . P(3) C(119) C(120) 117.8(4) yes . . . P(3) C(119) C(124) 122.9(5) yes . . . C(120) C(119) C(124) 119.3(6) yes . . . C(119) C(120) C(121) 119.5(6) yes . . . C(120) C(121) C(122) 120.2(8) yes . . . C(121) C(122) C(123) 121.3(8) yes . . . C(122) C(123) C(124) 119.8(8) yes . . . C(119) C(124) C(123) 119.9(7) yes . . . P(4) C(125) C(126) 118.9(4) yes . . . P(4) C(125) C(130) 121.8(4) yes . . . C(126) C(125) C(130) 119.3(5) yes . . . C(125) C(126) C(127) 119.9(5) yes . . . C(126) C(127) C(128) 120.9(6) yes . . . C(127) C(128) C(129) 119.2(6) yes . . . C(128) C(129) C(130) 120.2(6) yes . . . C(125) C(130) C(129) 120.4(6) yes . . . P(4) C(131) C(132) 117.2(5) yes . . . P(4) C(131) C(136) 124.6(4) yes . . . C(132) C(131) C(136) 117.9(5) yes . . . C(131) C(132) C(133) 121.2(7) yes . . . C(132) C(133) C(134) 120.2(7) yes . . . C(133) C(134) C(135) 120.4(7) yes . . . C(134) C(135) C(136) 119.9(9) yes . . . C(131) C(136) C(135) 120.3(7) yes . . . P(5) C(201) C(202) 118.0(4) yes . . . P(5) C(201) C(206) 122.9(4) yes . . . C(202) C(201) C(206) 119.1(5) yes . . . C(201) C(202) C(203) 119.9(5) yes . . . C(202) C(203) C(204) 120.6(6) yes . . . C(203) C(204) C(205) 120.2(6) yes . . . C(204) C(205) C(206) 119.6(6) yes . . . C(201) C(206) C(205) 120.6(5) yes . . . P(5) C(207) C(208) 124.8(3) yes . . . P(5) C(207) C(212) 116.1(4) yes . . . C(208) C(207) C(212) 119.1(5) yes . . . C(207) C(208) C(209) 120.8(4) yes . . . C(208) C(209) C(210) 120.1(6) yes . . . C(209) C(210) C(211) 119.9(7) yes . . . C(210) C(211) C(212) 120.3(6) yes . . . C(207) C(212) C(211) 119.7(6) yes . . . P(6) C(213) C(214) 117.6(4) yes . . . P(6) C(213) C(218) 122.8(4) yes . . . C(214) C(213) C(218) 119.5(5) yes . . . C(213) C(214) C(215) 119.8(5) yes . . . C(214) C(215) C(216) 120.2(6) yes . . . C(215) C(216) C(217) 120.2(6) yes . . . C(216) C(217) C(218) 119.9(5) yes . . . C(213) C(218) C(217) 120.3(5) yes . . . P(7) C(219) C(220) 118.4(4) yes . . . P(7) C(219) C(224) 122.3(4) yes . . . C(220) C(219) C(224) 119.3(5) yes . . . C(219) C(220) C(221) 119.9(5) yes . . . C(220) C(221) C(222) 120.2(6) yes . . . C(221) C(222) C(223) 120.3(6) yes . . . C(222) C(223) C(224) 120.1(6) yes . . . C(219) C(224) C(223) 120.1(5) yes . . . P(8) C(225) C(226) 118.7(4) yes . . . P(8) C(225) C(230) 122.4(4) yes . . . C(226) C(225) C(230) 118.9(5) yes . . . C(225) C(226) C(227) 120.4(6) yes . . . C(226) C(227) C(228) 120.4(7) yes . . . C(227) C(228) C(229) 119.6(7) yes . . . C(228) C(229) C(230) 120.6(6) yes . . . C(225) C(230) C(229) 120.0(6) yes . . . P(8) C(231) C(232) 116.1(5) yes . . . P(8) C(231) C(236) 125.0(4) yes . . . C(232) C(231) C(236) 118.9(6) yes . . . C(231) C(232) C(233) 120.5(9) yes . . . C(232) C(233) C(234) 121.3(9) yes . . . C(233) C(234) C(235) 119.3(9) yes . . . C(234) C(235) C(236) 119.9(10) yes . . . C(231) C(236) C(235) 119.9(7) yes . . . P(1) C(1) H(1) 108.5 no . . . P(1) C(1) H(2) 108.5 no . . . P(2) C(1) H(1) 108.7 no . . . P(2) C(1) H(2) 108.6 no . . . H(1) C(1) H(2) 109.6 no . . . P(2) C(2) H(3) 108.1 no . . . P(2) C(2) H(4) 108.2 no . . . P(3) C(2) H(3) 108.2 no . . . P(3) C(2) H(4) 108.3 no . . . H(3) C(2) H(4) 109.8 no . . . P(3) C(3) H(5) 108.4 no . . . P(3) C(3) H(6) 109.1 no . . . P(4) C(3) H(5) 108.9 no . . . P(4) C(3) H(6) 109.6 no . . . H(5) C(3) H(6) 108.9 no . . . P(5) C(4) H(7) 108.9 no . . . P(5) C(4) H(8) 108.5 no . . . P(6) C(4) H(7) 109.5 no . . . P(6) C(4) H(8) 109.1 no . . . H(7) C(4) H(8) 109.0 no . . . P(6) C(5) H(9) 108.1 no . . . P(6) C(5) H(10) 108.2 no . . . P(7) C(5) H(9) 108.5 no . . . P(7) C(5) H(10) 108.6 no . . . H(9) C(5) H(10) 108.7 no . . . P(7) C(6) H(11) 108.7 no . . . P(7) C(6) H(12) 108.5 no . . . P(8) C(6) H(11) 108.7 no . . . P(8) C(6) H(12) 108.4 no . . . H(11) C(6) H(12) 109.3 no . . . O(1) C(11) H(25) 118.3 no . . . N(1) C(11) H(25) 118.0 no . . . N(1) C(12) H(13) 109.2 no . . . N(1) C(12) H(14) 110.5 no . . . N(1) C(12) H(15) 110.5 no . . . H(13) C(12) H(14) 108.5 no . . . H(13) C(12) H(15) 108.8 no . . . H(14) C(12) H(15) 109.3 no . . . N(1) C(13) H(16) 109.0 no . . . N(1) C(13) H(17) 110.6 no . . . N(1) C(13) H(18) 111.3 no . . . H(16) C(13) H(17) 108.1 no . . . H(16) C(13) H(18) 108.0 no . . . H(17) C(13) H(18) 109.8 no . . . O(2) C(21) H(26) 118.5 no . . . N(2) C(21) H(26) 117.2 no . . . N(2) C(22) H(19) 109.7 no . . . N(2) C(22) H(20) 109.3 no . . . N(2) C(22) H(21) 110.1 no . . . H(19) C(22) H(20) 108.9 no . . . H(19) C(22) H(21) 109.6 no . . . H(20) C(22) H(21) 109.2 no . . . N(2) C(23) H(22) 109.9 no . . . N(2) C(23) H(23) 111.0 no . . . N(2) C(23) H(24) 111.3 no . . . H(22) C(23) H(23) 107.6 no . . . H(22) C(23) H(24) 107.6 no . . . H(23) C(23) H(24) 109.4 no . . . O(11) C(31) H(111) 147.7 no . . . N(11) C(31) H(111) 110.2 no . . . N(11) C(32) H(87) 111.8 no . . . N(11) C(32) H(88) 112.4 no . . . N(11) C(32) H(89) 108.4 no . . . H(87) C(32) H(88) 110.9 no . . . H(87) C(32) H(89) 106.3 no . . . H(88) C(32) H(89) 106.8 no . . . N(11) C(33) H(90) 112.1 no . . . N(11) C(33) H(91) 112.8 no . . . N(11) C(33) H(92) 108.9 no . . . H(90) C(33) H(91) 111.1 no . . . H(90) C(33) H(92) 105.2 no . . . H(91) C(33) H(92) 106.3 no . . . O(12) C(34) H(112) 120.2 no . . . N(12) C(34) H(112) 125.7 no . . . N(12) C(35) H(93) 115.7 no . . . N(12) C(35) H(94) 104.9 no . . . N(12) C(35) H(95) 109.9 no . . . H(93) C(35) H(94) 108.9 no . . . H(93) C(35) H(95) 113.5 no . . . H(94) C(35) H(95) 102.8 no . . . N(12) C(36) H(96) 111.0 no . . . N(12) C(36) H(97) 110.3 no . . . N(12) C(36) H(98) 111.7 no . . . H(96) C(36) H(97) 107.8 no . . . H(96) C(36) H(98) 109.1 no . . . H(97) C(36) H(98) 106.8 no . . . O(13) C(37) H(113) 121.8 no . . . N(13) C(37) H(113) 111.9 no . . . N(13) C(38) H(99) 106.0 no . . . N(13) C(38) H(100) 103.4 no . . . N(13) C(38) H(101) 126.4 no . . . H(99) C(38) H(100) 90.0 no . . . H(99) C(38) H(101) 115.4 no . . . H(100) C(38) H(101) 108.8 no . . . N(13) C(39) H(102) 104.2 no . . . N(13) C(39) H(103) 100.0 no . . . N(13) C(39) H(104) 116.1 no . . . H(102) C(39) H(103) 98.0 no . . . H(102) C(39) H(104) 122.2 no . . . H(103) C(39) H(104) 112.7 no . . . O(14) C(40) H(114) 124.1 no . . . N(14) C(40) H(114) 112.3 no . . . N(14) C(41) H(105) 109.3 no . . . N(14) C(41) H(106) 124.2 no . . . N(14) C(41) H(107) 120.9 no . . . H(105) C(41) H(106) 91.2 no . . . H(105) C(41) H(107) 93.9 no . . . H(106) C(41) H(107) 108.1 no . . . N(14) C(42) H(108) 115.3 no . . . N(14) C(42) H(109) 114.7 no . . . N(14) C(42) H(110) 112.3 no . . . H(108) C(42) H(109) 101.9 no . . . H(108) C(42) H(110) 109.8 no . . . H(109) C(42) H(110) 101.6 no . . . C(101) C(102) H(27) 119.9 no . . . C(103) C(102) H(27) 119.7 no . . . C(102) C(103) H(28) 119.0 no . . . C(104) C(103) H(28) 120.5 no . . . C(103) C(104) H(29) 119.5 no . . . C(105) C(104) H(29) 120.6 no . . . C(104) C(105) H(30) 120.2 no . . . C(106) C(105) H(30) 119.9 no . . . C(101) C(106) H(31) 119.1 no . . . C(105) C(106) H(31) 119.8 no . . . C(107) C(108) H(32) 120.1 no . . . C(109) C(108) H(32) 119.9 no . . . C(108) C(109) H(33) 119.4 no . . . C(110) C(109) H(33) 119.5 no . . . C(109) C(110) H(34) 120.6 no . . . C(111) C(110) H(34) 120.1 no . . . C(110) C(111) H(35) 119.9 no . . . C(112) C(111) H(35) 120.1 no . . . C(107) C(112) H(36) 119.4 no . . . C(111) C(112) H(36) 119.7 no . . . C(113) C(114) H(37) 120.4 no . . . C(115) C(114) H(37) 119.6 no . . . C(114) C(115) H(38) 119.9 no . . . C(116) C(115) H(38) 120.0 no . . . C(115) C(116) H(39) 120.2 no . . . C(117) C(116) H(39) 119.7 no . . . C(116) C(117) H(40) 119.5 no . . . C(118) C(117) H(40) 120.0 no . . . C(113) C(118) H(41) 120.1 no . . . C(117) C(118) H(41) 120.0 no . . . C(119) C(120) H(42) 119.9 no . . . C(121) C(120) H(42) 120.6 no . . . C(120) C(121) H(43) 119.4 no . . . C(122) C(121) H(43) 120.4 no . . . C(121) C(122) H(44) 119.7 no . . . C(123) C(122) H(44) 119.0 no . . . C(122) C(123) H(45) 119.4 no . . . C(124) C(123) H(45) 120.8 no . . . C(119) C(124) H(46) 119.5 no . . . C(123) C(124) H(46) 120.6 no . . . C(125) C(126) H(47) 119.5 no . . . C(127) C(126) H(47) 120.6 no . . . C(126) C(127) H(48) 119.5 no . . . C(128) C(127) H(48) 119.6 no . . . C(127) C(128) H(49) 120.3 no . . . C(129) C(128) H(49) 120.4 no . . . C(128) C(129) H(50) 118.8 no . . . C(130) C(129) H(50) 121.0 no . . . C(125) C(130) H(51) 119.9 no . . . C(129) C(130) H(51) 119.7 no . . . C(131) C(132) H(52) 118.6 no . . . C(133) C(132) H(52) 120.2 no . . . C(132) C(133) H(53) 120.2 no . . . C(134) C(133) H(53) 119.6 no . . . C(133) C(134) H(54) 120.3 no . . . C(135) C(134) H(54) 119.3 no . . . C(134) C(135) H(55) 120.8 no . . . C(136) C(135) H(55) 119.3 no . . . C(131) C(136) H(56) 119.3 no . . . C(135) C(136) H(56) 120.4 no . . . C(201) C(202) H(57) 120.0 no . . . C(203) C(202) H(57) 120.0 no . . . C(202) C(203) H(58) 119.5 no . . . C(204) C(203) H(58) 120.0 no . . . C(203) C(204) H(59) 119.8 no . . . C(205) C(204) H(59) 120.0 no . . . C(204) C(205) H(60) 119.7 no . . . C(206) C(205) H(60) 120.8 no . . . C(201) C(206) H(61) 120.0 no . . . C(205) C(206) H(61) 119.5 no . . . C(207) C(208) H(62) 119.1 no . . . C(209) C(208) H(62) 120.2 no . . . C(208) C(209) H(63) 119.3 no . . . C(210) C(209) H(63) 120.6 no . . . C(209) C(210) H(64) 120.3 no . . . C(211) C(210) H(64) 119.7 no . . . C(210) C(211) H(65) 120.2 no . . . C(212) C(211) H(65) 119.5 no . . . C(207) C(212) H(66) 119.7 no . . . C(211) C(212) H(66) 120.6 no . . . C(213) C(214) H(67) 119.6 no . . . C(215) C(214) H(67) 120.6 no . . . C(214) C(215) H(68) 119.8 no . . . C(216) C(215) H(68) 120.1 no . . . C(215) C(216) H(69) 119.6 no . . . C(217) C(216) H(69) 120.2 no . . . C(216) C(217) H(70) 120.1 no . . . C(218) C(217) H(70) 120.0 no . . . C(213) C(218) H(71) 119.4 no . . . C(217) C(218) H(71) 120.3 no . . . C(219) C(220) H(72) 119.6 no . . . C(221) C(220) H(72) 120.4 no . . . C(220) C(221) H(73) 119.6 no . . . C(222) C(221) H(73) 120.2 no . . . C(221) C(222) H(74) 120.3 no . . . C(223) C(222) H(74) 119.4 no . . . C(222) C(223) H(75) 120.4 no . . . C(224) C(223) H(75) 119.4 no . . . C(219) C(224) H(76) 120.0 no . . . C(223) C(224) H(76) 119.9 no . . . C(225) C(226) H(77) 119.9 no . . . C(227) C(226) H(77) 119.7 no . . . C(226) C(227) H(78) 118.5 no . . . C(228) C(227) H(78) 121.0 no . . . C(227) C(228) H(79) 120.2 no . . . C(229) C(228) H(79) 120.2 no . . . C(228) C(229) H(80) 120.0 no . . . C(230) C(229) H(80) 119.4 no . . . C(225) C(230) H(81) 119.6 no . . . C(229) C(230) H(81) 120.4 no . . . C(231) C(232) H(82) 119.2 no . . . C(233) C(232) H(82) 120.3 no . . . C(232) C(233) H(83) 119.1 no . . . C(234) C(233) H(83) 119.6 no . . . C(233) C(234) H(84) 122.1 no . . . C(235) C(234) H(84) 118.5 no . . . C(234) C(235) H(85) 120.4 no . . . C(236) C(235) H(85) 119.7 no . . . C(231) C(236) H(86) 120.2 no . . . C(235) C(236) H(86) 119.8 no . . . #============================================================================== data__compound5-revised #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731699' # CHEMICAL DATA _chemical_formula_sum 'C92 H90 Cl8 Cu4 I4 N2 P8 ' _chemical_formula_moiety 'C92 H90 Cl8 Cu4 I4 N2 P8 ' _chemical_formula_weight 2516.95 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 15.187(6) _cell_length_b 20.986(7) _cell_length_c 33.433(13) _cell_angle_alpha 90.0000 _cell_angle_beta 101.688(6) _cell_angle_gamma 90.0000 _cell_volume 10435(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12344 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4960.00 _exptl_absorpt_coefficient_mu 2.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.702 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 47987 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 42 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11550 _reflns_number_gt 9952 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1654 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 11550 _refine_ls_number_parameters 561 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0976P)^2^+89.3988P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 2.73 _refine_diff_density_min -1.44 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 1.03597(2) 0.009340(15) 0.874430(9) 0.03358(13) Uani 1.00 1 d . . . I(2) I 1.0000 -0.02600(2) 0.7500 0.03463(14) Uani 1.00 2 d S . . I(3) I 0.98864(12) 0.32481(4) 0.75821(5) 0.0606(4) Uani 0.50 1 d P . . Cu(1) Cu 1.03662(3) 0.12869(2) 0.904350(16) 0.02537(14) Uani 1.00 1 d . . . Cu(2) Cu 1.01353(3) 0.07202(2) 0.802800(16) 0.02548(14) Uani 1.00 1 d . . . Cl(1) Cl 1.3616(2) 0.29345(16) 0.55709(14) 0.1290(14) Uani 1.00 1 d . . . Cl(2) Cl 1.2987(2) 0.40091(16) 0.50647(10) 0.1117(10) Uani 1.00 1 d . . . Cl(3) Cl 0.9949(3) -0.2413(3) 0.8409(2) 0.130(3) Uani 0.50 1 d PD . . Cl(4) Cl 0.8565(2) -0.1616(2) 0.84538(13) 0.0745(10) Uani 0.50 1 d PD . . Cl(5) Cl 1.6970(3) 0.3441(2) 0.83174(17) 0.0835(13) Uani 0.50 1 d PD . . Cl(6) Cl 1.6538(3) 0.2818(2) 0.75763(14) 0.0831(12) Uani 0.50 1 d PD . . P(1) P 1.15311(7) 0.18438(5) 0.88935(3) 0.0238(2) Uani 1.00 1 d . . . P(2) P 1.14127(7) 0.12586(5) 0.80227(3) 0.0232(2) Uani 1.00 1 d . . . P(3) P 1.11873(7) 0.12397(5) 0.70656(3) 0.0225(2) Uani 1.00 1 d . . . P(4) P 1.09713(7) 0.17611(5) 0.61773(3) 0.0222(2) Uani 1.00 1 d . . . N(1) N 1.0617(2) 0.1120(2) 0.96728(12) 0.0319(7) Uani 1.00 1 d . . . C(1) C 1.1561(2) 0.1968(2) 0.83536(13) 0.0264(8) Uani 1.00 1 d . . . C(2) C 1.1475(3) 0.1691(2) 0.75467(13) 0.0267(8) Uani 1.00 1 d . . . C(3) C 1.1252(2) 0.1929(2) 0.67271(13) 0.0258(7) Uani 1.00 1 d . . . C(4) C 1.0540(3) 0.1575(2) 0.99381(16) 0.0383(10) Uani 1.00 1 d . . . C(5) C 1.0699(4) 0.1482(3) 1.03593(17) 0.0444(12) Uani 1.00 1 d . . . C(6) C 1.0939(4) 0.0884(3) 1.05147(16) 0.0493(13) Uani 1.00 1 d . . . C(7) C 1.1016(7) 0.0418(3) 1.0244(2) 0.075(2) Uani 1.00 1 d . . . C(8) C 1.0853(6) 0.0550(2) 0.98288(19) 0.0596(18) Uani 1.00 1 d . . . C(9) C 1.1587(2) 0.2662(2) 0.90822(13) 0.0266(8) Uani 1.00 1 d . . . C(10) C 1.1439(4) 0.3196(2) 0.88306(16) 0.0422(11) Uani 1.00 1 d . . . C(11) C 1.1426(5) 0.3804(2) 0.90010(19) 0.0542(15) Uani 1.00 1 d . . . C(12) C 1.1585(4) 0.3883(2) 0.94181(18) 0.0456(12) Uani 1.00 1 d . . . C(13) C 1.1745(3) 0.3361(2) 0.96749(16) 0.0379(10) Uani 1.00 1 d . . . C(14) C 1.1738(3) 0.2756(2) 0.95084(14) 0.0325(9) Uani 1.00 1 d . . . C(15) C 1.2651(3) 0.1540(2) 0.91175(13) 0.0295(8) Uani 1.00 1 d . . . C(16) C 1.3408(3) 0.1935(2) 0.91778(16) 0.0379(10) Uani 1.00 1 d . . . C(17) C 1.4250(3) 0.1686(3) 0.93498(17) 0.0451(12) Uani 1.00 1 d . . . C(18) C 1.4334(3) 0.1058(3) 0.94594(19) 0.0514(15) Uani 1.00 1 d . . . C(19) C 1.3602(4) 0.0669(3) 0.9392(2) 0.0501(13) Uani 1.00 1 d . . . C(20) C 1.2745(3) 0.0900(2) 0.92258(17) 0.0388(10) Uani 1.00 1 d . . . C(21) C 1.2491(2) 0.0846(2) 0.81491(13) 0.0295(8) Uani 1.00 1 d . . . C(22) C 1.3302(3) 0.1179(3) 0.82092(17) 0.0398(11) Uani 1.00 1 d . . . C(23) C 1.4114(3) 0.0851(3) 0.83062(19) 0.0499(14) Uani 1.00 1 d . . . C(24) C 1.4113(4) 0.0198(4) 0.8330(2) 0.0577(17) Uani 1.00 1 d . . . C(25) C 1.3315(4) -0.0139(3) 0.8269(2) 0.0584(16) Uani 1.00 1 d . . . C(26) C 1.2500(3) 0.0188(2) 0.81804(18) 0.0408(11) Uani 1.00 1 d . . . C(27) C 1.2199(2) 0.0771(2) 0.70618(13) 0.0284(8) Uani 1.00 1 d . . . C(28) C 1.3046(3) 0.1051(2) 0.71219(16) 0.0397(11) Uani 1.00 1 d . . . C(29) C 1.3807(3) 0.0668(4) 0.7144(2) 0.0550(16) Uani 1.00 1 d . . . C(30) C 1.3725(4) 0.0012(4) 0.7111(2) 0.0581(17) Uani 1.00 1 d . . . C(31) C 1.2883(5) -0.0265(3) 0.7044(2) 0.0569(16) Uani 1.00 1 d . . . C(32) C 1.2125(3) 0.0117(2) 0.70160(18) 0.0405(11) Uani 1.00 1 d . . . C(33) C 1.1994(2) 0.1384(2) 0.60892(13) 0.0269(8) Uani 1.00 1 d . . . C(34) C 1.2787(3) 0.1712(2) 0.61105(16) 0.0365(10) Uani 1.00 1 d . . . C(35) C 1.3566(3) 0.1387(3) 0.6055(2) 0.0477(13) Uani 1.00 1 d . . . C(36) C 1.3533(4) 0.0743(3) 0.5984(2) 0.0515(14) Uani 1.00 1 d . . . C(37) C 1.2737(4) 0.0416(3) 0.5964(2) 0.0518(14) Uani 1.00 1 d . . . C(38) C 1.1972(3) 0.0731(2) 0.60158(17) 0.0377(10) Uani 1.00 1 d . . . C(39) C 1.1020(3) 0.2541(2) 0.59394(14) 0.0284(8) Uani 1.00 1 d . . . C(40) C 1.0814(4) 0.3105(2) 0.61154(17) 0.0424(11) Uani 1.00 1 d . . . C(41) C 1.0772(5) 0.3673(2) 0.5898(2) 0.0607(18) Uani 1.00 1 d . . . C(42) C 1.0928(5) 0.3677(3) 0.5505(2) 0.0578(17) Uani 1.00 1 d . . . C(43) C 1.1137(4) 0.3130(3) 0.53286(19) 0.0515(14) Uani 1.00 1 d . . . C(44) C 1.1186(3) 0.2556(2) 0.55404(16) 0.0381(10) Uani 1.00 1 d . . . C(101) C 1.3332(6) 0.3756(5) 0.5535(4) 0.104(4) Uani 1.00 1 d . . . C(102) C 0.9617(9) -0.1654(6) 0.8336(6) 0.073(4) Uani 0.50 1 d PD . . C(103) C 1.7107(14) 0.3473(8) 0.7803(4) 0.089(5) Uiso 0.50 1 d PD . . H(1) H 1.1095 0.2261 0.8246 0.033 Uiso 1.00 1 c R . . H(2) H 1.2127 0.2151 0.8342 0.033 Uiso 1.00 1 c R . . H(3) H 1.0849 0.2247 0.6785 0.031 Uiso 1.00 1 c R . . H(4) H 1.1850 0.2090 0.6790 0.031 Uiso 1.00 1 c R . . H(5) H 1.0365 0.1991 0.9834 0.046 Uiso 1.00 1 c R . . H(6) H 1.0632 0.1830 1.0538 0.054 Uiso 1.00 1 c R . . H(7) H 1.1042 0.0796 1.0800 0.061 Uiso 1.00 1 c R . . H(8) H 1.1214 0.0002 1.0343 0.089 Uiso 1.00 1 c R . . H(9) H 1.0901 0.0205 0.9645 0.072 Uiso 1.00 1 c R . . H(10) H 1.1346 0.3147 0.8542 0.050 Uiso 1.00 1 c R . . H(11) H 1.1293 0.4171 0.8828 0.064 Uiso 1.00 1 c R . . H(12) H 1.1594 0.4300 0.9531 0.054 Uiso 1.00 1 c R . . H(13) H 1.1862 0.3417 0.9963 0.045 Uiso 1.00 1 c R . . H(14) H 1.1838 0.2396 0.9685 0.040 Uiso 1.00 1 c R . . H(15) H 1.3349 0.2372 0.9101 0.047 Uiso 1.00 1 c R . . H(16) H 1.4769 0.1950 0.9393 0.054 Uiso 1.00 1 c R . . H(17) H 1.4905 0.0905 0.9590 0.063 Uiso 1.00 1 c R . . H(18) H 1.3682 0.0223 0.9458 0.062 Uiso 1.00 1 c R . . H(19) H 1.2228 0.0629 0.9185 0.047 Uiso 1.00 1 c R . . H(20) H 1.3301 0.1636 0.8182 0.050 Uiso 1.00 1 c R . . H(21) H 1.4666 0.1082 0.8358 0.060 Uiso 1.00 1 c R . . H(22) H 1.4671 -0.0025 0.8391 0.068 Uiso 1.00 1 c R . . H(23) H 1.3320 -0.0600 0.8282 0.071 Uiso 1.00 1 c R . . H(24) H 1.1947 -0.0039 0.8144 0.051 Uiso 1.00 1 c R . . H(25) H 1.3109 0.1506 0.7147 0.047 Uiso 1.00 1 c R . . H(26) H 1.4388 0.0850 0.7178 0.066 Uiso 1.00 1 c R . . H(27) H 1.4245 -0.0247 0.7133 0.070 Uiso 1.00 1 c R . . H(28) H 1.2832 -0.0712 0.7023 0.071 Uiso 1.00 1 c R . . H(29) H 1.1541 -0.0078 0.6955 0.050 Uiso 1.00 1 c R . . H(30) H 1.2814 0.2156 0.6169 0.044 Uiso 1.00 1 c R . . H(31) H 1.4111 0.1614 0.6061 0.057 Uiso 1.00 1 c R . . H(32) H 1.4065 0.0531 0.5948 0.063 Uiso 1.00 1 c R . . H(33) H 1.2707 -0.0032 0.5905 0.064 Uiso 1.00 1 c R . . H(34) H 1.1421 0.0498 0.6005 0.047 Uiso 1.00 1 c R . . H(35) H 1.0701 0.3103 0.6386 0.051 Uiso 1.00 1 c R . . H(36) H 1.0627 0.4060 0.6016 0.072 Uiso 1.00 1 c R . . H(37) H 1.0898 0.4073 0.5360 0.069 Uiso 1.00 1 c R . . H(38) H 1.1244 0.3132 0.5055 0.062 Uiso 1.00 1 c R . . H(39) H 1.1339 0.2174 0.5414 0.046 Uiso 1.00 1 c R . . H(40) H 1.2871 0.3816 0.5701 0.100 Uiso 1.00 1 c R . . H(41) H 1.3854 0.3987 0.5680 0.100 Uiso 1.00 1 c R . . H(42) H 1.0024 -0.1390 0.8508 0.084 Uiso 0.50 1 c R . . H(43) H 0.9584 -0.1531 0.8056 0.084 Uiso 0.50 1 c R . . H(44) H 1.6855 0.3848 0.7665 0.110 Uiso 0.50 1 c R . . H(45) H 1.7724 0.3444 0.7781 0.110 Uiso 0.50 1 c R . . H(46) H 1.1076 0.2044 0.7526 0.032 Uiso 1.00 1 c R . . H(47) H 1.2074 0.1842 0.7572 0.032 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0432(2) 0.02993(19) 0.02654(19) 0.00096(11) 0.00440(13) 0.00204(10) I(2) 0.0488(2) 0.0267(2) 0.0283(2) 0.0000 0.00747(18) 0.0000 I(3) 0.0607(8) 0.0329(3) 0.0787(12) -0.0009(3) -0.0083(6) 0.0071(3) Cu(1) 0.0256(2) 0.0252(2) 0.0242(2) 0.00012(18) 0.00242(19) 0.00176(18) Cu(2) 0.0244(2) 0.0254(2) 0.0255(2) 0.00030(18) 0.00252(19) 0.00193(18) Cl(1) 0.1033(19) 0.101(2) 0.207(3) 0.0170(16) 0.089(2) 0.063(2) Cl(2) 0.130(2) 0.109(2) 0.0918(18) -0.0464(18) 0.0120(16) 0.0352(15) Cl(3) 0.065(2) 0.118(4) 0.196(7) -0.000(2) 0.003(3) 0.101(4) Cl(4) 0.068(2) 0.097(2) 0.060(2) -0.019(2) 0.0173(17) 0.0087(19) Cl(5) 0.070(2) 0.062(2) 0.112(3) 0.0131(17) 0.005(2) 0.035(2) Cl(6) 0.102(3) 0.069(2) 0.071(2) 0.033(2) -0.002(2) -0.0075(19) P(1) 0.0240(4) 0.0270(5) 0.0191(4) -0.0029(3) 0.0009(3) -0.0017(3) P(2) 0.0226(4) 0.0272(5) 0.0184(4) -0.0007(3) 0.0009(3) -0.0010(3) P(3) 0.0227(4) 0.0251(4) 0.0185(4) 0.0002(3) 0.0017(3) -0.0006(3) P(4) 0.0243(4) 0.0223(4) 0.0195(4) 0.0001(3) 0.0031(3) 0.0003(3) N(1) 0.0375(19) 0.0318(19) 0.0262(18) 0.0025(15) 0.0060(15) 0.0053(14) C(1) 0.0273(19) 0.031(2) 0.0204(19) -0.0021(15) 0.0033(15) -0.0028(15) C(2) 0.034(2) 0.0273(19) 0.0180(18) -0.0032(16) 0.0028(15) -0.0037(14) C(3) 0.0302(19) 0.0256(18) 0.0204(18) -0.0004(15) 0.0023(15) 0.0006(14) C(4) 0.042(2) 0.042(2) 0.030(2) 0.003(2) 0.0035(19) 0.0002(19) C(5) 0.046(2) 0.057(3) 0.030(2) -0.003(2) 0.007(2) -0.008(2) C(6) 0.060(3) 0.065(3) 0.021(2) -0.007(2) 0.003(2) 0.009(2) C(7) 0.147(8) 0.045(3) 0.031(3) 0.015(4) 0.011(3) 0.015(2) C(8) 0.111(5) 0.034(2) 0.031(2) 0.013(3) 0.009(3) 0.005(2) C(9) 0.0271(19) 0.031(2) 0.0218(19) -0.0074(15) 0.0050(15) -0.0051(15) C(10) 0.067(3) 0.033(2) 0.027(2) -0.010(2) 0.008(2) -0.0029(18) C(11) 0.092(4) 0.032(2) 0.039(3) -0.013(2) 0.013(3) -0.001(2) C(12) 0.064(3) 0.032(2) 0.044(2) -0.014(2) 0.016(2) -0.011(2) C(13) 0.050(2) 0.038(2) 0.028(2) -0.008(2) 0.013(2) -0.0089(19) C(14) 0.038(2) 0.036(2) 0.023(2) -0.0041(18) 0.0062(17) -0.0040(17) C(15) 0.029(2) 0.040(2) 0.0188(19) -0.0007(17) 0.0017(15) -0.0032(16) C(16) 0.027(2) 0.054(3) 0.032(2) -0.005(2) 0.0032(18) -0.001(2) C(17) 0.027(2) 0.071(3) 0.036(2) 0.000(2) 0.0016(19) -0.005(2) C(18) 0.032(2) 0.078(4) 0.039(2) 0.018(2) -0.005(2) -0.010(2) C(19) 0.047(3) 0.049(3) 0.048(3) 0.014(2) -0.007(2) -0.003(2) C(20) 0.039(2) 0.038(2) 0.035(2) 0.0041(19) -0.005(2) -0.0011(19) C(21) 0.0268(19) 0.042(2) 0.0183(18) 0.0028(17) 0.0003(15) -0.0010(16) C(22) 0.026(2) 0.057(3) 0.035(2) 0.001(2) 0.0022(18) -0.000(2) C(23) 0.026(2) 0.082(4) 0.040(2) 0.006(2) 0.002(2) 0.002(2) C(24) 0.036(2) 0.088(5) 0.047(3) 0.026(3) 0.005(2) 0.011(3) C(25) 0.057(3) 0.052(3) 0.064(4) 0.025(2) 0.006(3) 0.010(3) C(26) 0.036(2) 0.039(2) 0.045(2) 0.010(2) 0.004(2) 0.005(2) C(27) 0.0279(19) 0.037(2) 0.0197(19) 0.0049(16) 0.0026(15) 0.0028(15) C(28) 0.026(2) 0.056(3) 0.036(2) 0.002(2) 0.0058(18) -0.002(2) C(29) 0.024(2) 0.094(5) 0.047(3) 0.012(2) 0.005(2) 0.005(3) C(30) 0.045(3) 0.084(4) 0.047(3) 0.034(3) 0.015(2) 0.017(3) C(31) 0.066(4) 0.052(3) 0.058(3) 0.027(3) 0.026(3) 0.013(2) C(32) 0.042(2) 0.038(2) 0.042(2) 0.010(2) 0.011(2) 0.003(2) C(33) 0.0276(19) 0.033(2) 0.0201(19) 0.0017(16) 0.0039(15) 0.0011(15) C(34) 0.030(2) 0.042(2) 0.038(2) -0.0002(19) 0.0088(19) 0.003(2) C(35) 0.029(2) 0.066(3) 0.051(3) 0.007(2) 0.014(2) 0.013(2) C(36) 0.042(2) 0.065(3) 0.051(3) 0.022(2) 0.016(2) -0.002(2) C(37) 0.055(3) 0.045(3) 0.056(3) 0.018(2) 0.012(2) -0.006(2) C(38) 0.040(2) 0.033(2) 0.040(2) 0.0046(19) 0.008(2) -0.0062(19) C(39) 0.030(2) 0.0251(19) 0.028(2) -0.0020(15) -0.0012(16) 0.0029(15) C(40) 0.056(3) 0.032(2) 0.035(2) 0.006(2) 0.000(2) -0.0017(19) C(41) 0.084(4) 0.027(2) 0.059(4) 0.008(2) -0.012(3) 0.002(2) C(42) 0.071(4) 0.037(2) 0.055(3) -0.010(2) -0.011(3) 0.019(2) C(43) 0.060(3) 0.049(3) 0.041(3) -0.014(2) 0.000(2) 0.018(2) C(44) 0.040(2) 0.039(2) 0.034(2) -0.0037(19) 0.005(2) 0.0087(19) C(101) 0.058(4) 0.080(6) 0.170(12) -0.019(4) 0.015(5) -0.049(7) C(102) 0.068(9) 0.047(7) 0.104(13) -0.019(6) 0.017(8) 0.013(7) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Cu(1) 2.6963(12) yes . . I(1) Cu(2) 2.6928(12) yes . . I(2) Cu(2) 2.6913(12) yes . . I(2) Cu(2) 2.6913(12) yes . 2_756 I(3) I(3) 0.705(2) yes . 2_756 Cu(1) P(1) 2.2598(12) yes . . Cu(1) P(4) 2.2481(11) yes . 2_756 Cu(1) N(1) 2.091(3) yes . . Cu(2) P(2) 2.2483(11) yes . . Cu(2) P(3) 2.2509(11) yes . 2_756 Cl(1) C(101) 1.776(11) yes . . Cl(2) C(101) 1.641(14) yes . . Cl(3) C(102) 1.675(14) yes . . Cl(4) C(102) 1.724(16) yes . . Cl(5) C(103) 1.776(18) yes . . Cl(6) C(103) 1.717(18) yes . . P(1) C(1) 1.833(4) yes . . P(1) C(9) 1.826(4) yes . . P(1) C(15) 1.828(4) yes . . P(2) C(1) 1.842(4) yes . . P(2) C(2) 1.851(4) yes . . P(2) C(21) 1.824(4) yes . . P(3) C(2) 1.842(4) yes . . P(3) C(3) 1.851(4) yes . . P(3) C(27) 1.827(4) yes . . P(4) C(3) 1.835(4) yes . . P(4) C(33) 1.819(4) yes . . P(4) C(39) 1.829(4) yes . . N(1) C(4) 1.326(6) yes . . N(1) C(8) 1.324(7) yes . . C(4) C(5) 1.394(7) yes . . C(5) C(6) 1.377(9) yes . . C(6) C(7) 1.354(9) yes . . C(7) C(8) 1.388(9) yes . . C(9) C(10) 1.391(6) yes . . C(9) C(14) 1.411(6) yes . . C(10) C(11) 1.401(8) yes . . C(11) C(12) 1.376(8) yes . . C(12) C(13) 1.384(7) yes . . C(13) C(14) 1.384(7) yes . . C(15) C(16) 1.398(6) yes . . C(15) C(20) 1.390(7) yes . . C(16) C(17) 1.393(7) yes . . C(17) C(18) 1.367(10) yes . . C(18) C(19) 1.361(8) yes . . C(19) C(20) 1.395(7) yes . . C(21) C(22) 1.395(6) yes . . C(21) C(26) 1.384(7) yes . . C(22) C(23) 1.392(7) yes . . C(23) C(24) 1.374(11) yes . . C(24) C(25) 1.382(9) yes . . C(25) C(26) 1.394(9) yes . . C(27) C(28) 1.391(6) yes . . C(27) C(32) 1.383(7) yes . . C(28) C(29) 1.398(8) yes . . C(29) C(30) 1.384(11) yes . . C(30) C(31) 1.381(10) yes . . C(31) C(32) 1.390(9) yes . . C(33) C(34) 1.377(6) yes . . C(33) C(38) 1.391(6) yes . . C(34) C(35) 1.410(8) yes . . C(35) C(36) 1.371(9) yes . . C(36) C(37) 1.380(9) yes . . C(37) C(38) 1.378(8) yes . . C(39) C(40) 1.386(7) yes . . C(39) C(44) 1.407(7) yes . . C(40) C(41) 1.391(8) yes . . C(41) C(42) 1.381(11) yes . . C(42) C(43) 1.357(9) yes . . C(43) C(44) 1.391(8) yes . . C(1) H(1) 0.951 no . . C(1) H(2) 0.950 no . . C(2) H(46) 0.950 no . . C(2) H(47) 0.950 no . . C(3) H(3) 0.951 no . . C(3) H(4) 0.952 no . . C(4) H(5) 0.957 no . . C(5) H(6) 0.963 no . . C(6) H(7) 0.952 no . . C(7) H(8) 0.960 no . . C(8) H(9) 0.962 no . . C(10) H(10) 0.951 no . . C(11) H(11) 0.960 no . . C(12) H(12) 0.950 no . . C(13) H(13) 0.952 no . . C(14) H(14) 0.951 no . . C(16) H(15) 0.952 no . . C(17) H(16) 0.949 no . . C(18) H(17) 0.945 no . . C(19) H(18) 0.963 no . . C(20) H(19) 0.957 no . . C(22) H(20) 0.964 no . . C(23) H(21) 0.954 no . . C(24) H(22) 0.953 no . . C(25) H(23) 0.968 no . . C(26) H(24) 0.952 no . . C(28) H(25) 0.962 no . . C(29) H(26) 0.947 no . . C(30) H(27) 0.948 no . . C(31) H(28) 0.943 no . . C(32) H(29) 0.961 no . . C(34) H(30) 0.952 no . . C(35) H(31) 0.952 no . . C(36) H(32) 0.952 no . . C(37) H(33) 0.959 no . . C(38) H(34) 0.963 no . . C(40) H(35) 0.954 no . . C(41) H(36) 0.948 no . . C(42) H(37) 0.960 no . . C(43) H(38) 0.960 no . . C(44) H(39) 0.955 no . . C(101) H(40) 0.986 no . . C(101) H(41) 0.970 no . . C(102) H(42) 0.936 no . . C(102) H(43) 0.961 no . . C(103) H(44) 0.953 no . . C(103) H(45) 0.957 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) I(1) Cu(2) 82.325(17) yes . . . Cu(2) I(2) Cu(2) 80.302(18) yes . . 2_756 I(1) Cu(1) P(1) 110.02(3) yes . . . I(1) Cu(1) P(4) 110.75(3) yes . . 2_756 I(1) Cu(1) N(1) 101.75(11) yes . . . P(1) Cu(1) P(4) 113.21(4) yes . . 2_756 P(1) Cu(1) N(1) 108.59(11) yes . . . P(4) Cu(1) N(1) 111.92(12) yes 2_756 . . I(1) Cu(2) I(2) 100.898(16) yes . . . I(1) Cu(2) P(2) 107.37(3) yes . . . I(1) Cu(2) P(3) 107.99(3) yes . . 2_756 I(2) Cu(2) P(2) 109.29(3) yes . . . I(2) Cu(2) P(3) 109.37(3) yes . . 2_756 P(2) Cu(2) P(3) 120.18(4) yes . . 2_756 Cu(1) P(1) C(1) 117.93(14) yes . . . Cu(1) P(1) C(9) 113.19(15) yes . . . Cu(1) P(1) C(15) 115.70(16) yes . . . C(1) P(1) C(9) 101.4(2) yes . . . C(1) P(1) C(15) 104.3(2) yes . . . C(9) P(1) C(15) 102.24(19) yes . . . Cu(2) P(2) C(1) 113.70(15) yes . . . Cu(2) P(2) C(2) 116.60(13) yes . . . Cu(2) P(2) C(21) 119.67(16) yes . . . C(1) P(2) C(2) 95.66(19) yes . . . C(1) P(2) C(21) 104.48(19) yes . . . C(2) P(2) C(21) 103.4(2) yes . . . Cu(2) P(3) C(2) 114.70(15) yes 2_756 . . Cu(2) P(3) C(3) 116.72(13) yes 2_756 . . Cu(2) P(3) C(27) 117.79(15) yes 2_756 . . C(2) P(3) C(3) 95.70(19) yes . . . C(2) P(3) C(27) 103.42(19) yes . . . C(3) P(3) C(27) 105.5(2) yes . . . Cu(1) P(4) C(3) 115.14(15) yes 2_756 . . Cu(1) P(4) C(33) 119.88(14) yes 2_756 . . Cu(1) P(4) C(39) 111.54(13) yes 2_756 . . C(3) P(4) C(33) 102.31(19) yes . . . C(3) P(4) C(39) 104.01(19) yes . . . C(33) P(4) C(39) 102.0(2) yes . . . Cu(1) N(1) C(4) 122.0(3) yes . . . Cu(1) N(1) C(8) 121.9(3) yes . . . C(4) N(1) C(8) 116.2(4) yes . . . P(1) C(1) P(2) 116.9(2) yes . . . P(2) C(2) P(3) 117.0(2) yes . . . P(3) C(3) P(4) 115.6(2) yes . . . N(1) C(4) C(5) 123.6(5) yes . . . C(4) C(5) C(6) 119.2(5) yes . . . C(5) C(6) C(7) 117.2(5) yes . . . C(6) C(7) C(8) 120.1(6) yes . . . N(1) C(8) C(7) 123.6(6) yes . . . P(1) C(9) C(10) 123.9(3) yes . . . P(1) C(9) C(14) 117.9(3) yes . . . C(10) C(9) C(14) 118.1(4) yes . . . C(9) C(10) C(11) 120.1(4) yes . . . C(10) C(11) C(12) 120.5(5) yes . . . C(11) C(12) C(13) 120.4(5) yes . . . C(12) C(13) C(14) 119.4(4) yes . . . C(9) C(14) C(13) 121.4(4) yes . . . P(1) C(15) C(16) 121.5(3) yes . . . P(1) C(15) C(20) 118.8(3) yes . . . C(16) C(15) C(20) 119.8(4) yes . . . C(15) C(16) C(17) 119.8(5) yes . . . C(16) C(17) C(18) 119.9(5) yes . . . C(17) C(18) C(19) 120.4(5) yes . . . C(18) C(19) C(20) 121.5(5) yes . . . C(15) C(20) C(19) 118.6(5) yes . . . P(2) C(21) C(22) 121.4(4) yes . . . P(2) C(21) C(26) 119.0(3) yes . . . C(22) C(21) C(26) 119.6(4) yes . . . C(21) C(22) C(23) 120.1(5) yes . . . C(22) C(23) C(24) 119.7(5) yes . . . C(23) C(24) C(25) 120.9(6) yes . . . C(24) C(25) C(26) 119.6(6) yes . . . C(21) C(26) C(25) 120.1(5) yes . . . P(3) C(27) C(28) 121.7(3) yes . . . P(3) C(27) C(32) 119.1(3) yes . . . C(28) C(27) C(32) 119.2(4) yes . . . C(27) C(28) C(29) 119.6(5) yes . . . C(28) C(29) C(30) 120.5(5) yes . . . C(29) C(30) C(31) 119.8(6) yes . . . C(30) C(31) C(32) 119.7(6) yes . . . C(27) C(32) C(31) 121.1(5) yes . . . P(4) C(33) C(34) 122.7(3) yes . . . P(4) C(33) C(38) 117.8(3) yes . . . C(34) C(33) C(38) 119.4(4) yes . . . C(33) C(34) C(35) 119.9(5) yes . . . C(34) C(35) C(36) 119.8(5) yes . . . C(35) C(36) C(37) 120.0(6) yes . . . C(36) C(37) C(38) 120.5(5) yes . . . C(33) C(38) C(37) 120.3(5) yes . . . P(4) C(39) C(40) 123.2(4) yes . . . P(4) C(39) C(44) 117.6(3) yes . . . C(40) C(39) C(44) 118.9(4) yes . . . C(39) C(40) C(41) 120.0(5) yes . . . C(40) C(41) C(42) 120.3(6) yes . . . C(41) C(42) C(43) 120.5(6) yes . . . C(42) C(43) C(44) 120.3(6) yes . . . C(39) C(44) C(43) 120.0(5) yes . . . Cl(1) C(101) Cl(2) 113.9(8) yes . . . Cl(3) C(102) Cl(4) 106.0(8) yes . . . Cl(5) C(103) Cl(6) 104.4(10) yes . . . P(1) C(1) H(1) 107.6 no . . . P(1) C(1) H(2) 107.6 no . . . P(2) C(1) H(1) 107.6 no . . . P(2) C(1) H(2) 107.7 no . . . H(1) C(1) H(2) 109.4 no . . . P(2) C(2) H(46) 107.6 no . . . P(2) C(2) H(47) 107.6 no . . . P(3) C(2) H(46) 107.6 no . . . P(3) C(2) H(47) 107.6 no . . . H(46) C(2) H(47) 109.4 no . . . P(3) C(3) H(3) 108.0 no . . . P(3) C(3) H(4) 108.0 no . . . P(4) C(3) H(3) 108.0 no . . . P(4) C(3) H(4) 107.9 no . . . H(3) C(3) H(4) 109.2 no . . . N(1) C(4) H(5) 118.0 no . . . C(5) C(4) H(5) 118.4 no . . . C(4) C(5) H(6) 120.2 no . . . C(6) C(5) H(6) 120.6 no . . . C(5) C(6) H(7) 122.2 no . . . C(7) C(6) H(7) 120.6 no . . . C(6) C(7) H(8) 119.3 no . . . C(8) C(7) H(8) 120.5 no . . . N(1) C(8) H(9) 118.5 no . . . C(7) C(8) H(9) 117.8 no . . . C(9) C(10) H(10) 120.0 no . . . C(11) C(10) H(10) 119.9 no . . . C(10) C(11) H(11) 120.4 no . . . C(12) C(11) H(11) 119.1 no . . . C(11) C(12) H(12) 119.9 no . . . C(13) C(12) H(12) 119.7 no . . . C(12) C(13) H(13) 120.2 no . . . C(14) C(13) H(13) 120.4 no . . . C(9) C(14) H(14) 119.2 no . . . C(13) C(14) H(14) 119.4 no . . . C(15) C(16) H(15) 120.1 no . . . C(17) C(16) H(15) 120.0 no . . . C(16) C(17) H(16) 120.6 no . . . C(18) C(17) H(16) 119.5 no . . . C(17) C(18) H(17) 118.6 no . . . C(19) C(18) H(17) 121.0 no . . . C(18) C(19) H(18) 119.0 no . . . C(20) C(19) H(18) 119.5 no . . . C(15) C(20) H(19) 120.0 no . . . C(19) C(20) H(19) 121.5 no . . . C(21) C(22) H(20) 120.0 no . . . C(23) C(22) H(20) 119.9 no . . . C(22) C(23) H(21) 119.7 no . . . C(24) C(23) H(21) 120.5 no . . . C(23) C(24) H(22) 119.3 no . . . C(25) C(24) H(22) 119.8 no . . . C(24) C(25) H(23) 120.3 no . . . C(26) C(25) H(23) 120.0 no . . . C(21) C(26) H(24) 119.6 no . . . C(25) C(26) H(24) 120.2 no . . . C(27) C(28) H(25) 120.4 no . . . C(29) C(28) H(25) 120.0 no . . . C(28) C(29) H(26) 120.9 no . . . C(30) C(29) H(26) 118.5 no . . . C(29) C(30) H(27) 120.2 no . . . C(31) C(30) H(27) 120.0 no . . . C(30) C(31) H(28) 119.4 no . . . C(32) C(31) H(28) 120.9 no . . . C(27) C(32) H(29) 119.8 no . . . C(31) C(32) H(29) 119.1 no . . . C(33) C(34) H(30) 120.1 no . . . C(35) C(34) H(30) 119.9 no . . . C(34) C(35) H(31) 120.4 no . . . C(36) C(35) H(31) 119.8 no . . . C(35) C(36) H(32) 118.8 no . . . C(37) C(36) H(32) 121.2 no . . . C(36) C(37) H(33) 120.2 no . . . C(38) C(37) H(33) 119.2 no . . . C(33) C(38) H(34) 119.7 no . . . C(37) C(38) H(34) 120.1 no . . . C(39) C(40) H(35) 119.8 no . . . C(41) C(40) H(35) 120.2 no . . . C(40) C(41) H(36) 120.4 no . . . C(42) C(41) H(36) 119.3 no . . . C(41) C(42) H(37) 119.1 no . . . C(43) C(42) H(37) 120.3 no . . . C(42) C(43) H(38) 120.5 no . . . C(44) C(43) H(38) 119.2 no . . . C(39) C(44) H(39) 120.4 no . . . C(43) C(44) H(39) 119.6 no . . . Cl(1) C(101) H(40) 106.0 no . . . Cl(1) C(101) H(41) 106.7 no . . . Cl(2) C(101) H(40) 111.9 no . . . Cl(2) C(101) H(41) 112.8 no . . . H(40) C(101) H(41) 104.9 no . . . Cl(3) C(102) H(42) 109.4 no . . . Cl(3) C(102) H(43) 110.7 no . . . Cl(4) C(102) H(42) 111.0 no . . . Cl(4) C(102) H(43) 110.0 no . . . H(42) C(102) H(43) 109.7 no . . . Cl(5) C(103) H(44) 112.6 no . . . Cl(5) C(103) H(45) 112.4 no . . . Cl(6) C(103) H(44) 109.4 no . . . Cl(6) C(103) H(45) 109.2 no . . . H(44) C(103) H(45) 108.7 no . . . #============================================================================== #============================================================================== data__compound6a-revised #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731700' # CHEMICAL DATA _chemical_formula_sum 'C98 H94 Cl7 Cu4 F6 N2 P9 ' _chemical_formula_moiety 'C98 H94 Cl7 Cu4 F6 N2 P9 ' _chemical_formula_weight 2194.94 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 18.4639(5) _cell_length_b 26.5980(5) _cell_length_c 20.4810(5) _cell_angle_alpha 90.0000 _cell_angle_beta 94.8073(5) _cell_angle_gamma 90.0000 _cell_volume 10022.9(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20479 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480.00 _exptl_absorpt_coefficient_mu 1.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.736 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 94792 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 22361 _reflns_number_gt 15848 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1151 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 22361 _refine_ls_number_parameters 1156 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0594P)^2^+25.0551P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 1.32 _refine_diff_density_min -1.29 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.68587(2) 0.038550(15) 0.30439(2) 0.02483(11) Uani 1.00 1 d . . . Cu(2) Cu 0.57929(2) 0.140010(15) 0.34926(2) 0.02360(10) Uani 1.00 1 d . . . Cu(3) Cu 0.46467(2) 0.236530(16) 0.34487(2) 0.02335(10) Uani 1.00 1 d . . . Cu(4) Cu 0.35156(2) 0.333260(15) 0.30013(2) 0.02219(10) Uani 1.00 1 d . . . Cl(1) Cl 0.66227(5) 0.07991(3) 0.40418(4) 0.02731(17) Uani 1.00 1 d . . . Cl(2) Cl 0.52789(5) 0.18968(3) 0.43168(4) 0.02701(17) Uani 1.00 1 d . . . Cl(3) Cl 0.40731(5) 0.30318(3) 0.40147(4) 0.02816(17) Uani 1.00 1 d . . . Cl(11) Cl 0.06706(13) 0.91522(9) 0.97927(12) 0.1143(7) Uani 1.00 1 d D . . Cl(12) Cl -0.0648(2) 0.8743(2) 0.9130(2) 0.185(3) Uani 0.72(8) 1 d PD . . Cl(13) Cl -0.0873(5) 0.9293(4) 0.9607(5) 0.132(5) Uani 0.28(8) 1 d PD . . Cl(14) Cl 0.1944(2) 0.76750(12) 0.94139(17) 0.1537(11) Uani 1.00 1 d D . . Cl(15) Cl 0.035(2) 0.7626(8) 0.8796(15) 0.201(15) Uani 0.47(4) 1 d PD . . Cl(16) Cl 0.0742(6) 0.7496(4) 0.8625(4) 0.118(3) Uani 0.53(4) 1 d PD . . P(1) P 0.57926(5) 0.00665(3) 0.26021(4) 0.02232(17) Uani 1.00 1 d . . . P(2) P 0.48400(4) 0.09540(3) 0.30380(4) 0.01911(16) Uani 1.00 1 d . . . P(3) P 0.37750(4) 0.18600(3) 0.29915(4) 0.01906(16) Uani 1.00 1 d . . . P(4) P 0.27801(4) 0.27413(3) 0.25025(4) 0.02027(16) Uani 1.00 1 d . . . P(5) P 0.73477(5) 0.09428(3) 0.23645(4) 0.02303(17) Uani 1.00 1 d . . . P(6) P 0.65199(4) 0.18622(3) 0.28925(4) 0.02016(16) Uani 1.00 1 d . . . P(7) P 0.54661(4) 0.27758(3) 0.28927(4) 0.01951(16) Uani 1.00 1 d . . . P(8) P 0.43967(4) 0.36168(3) 0.23898(4) 0.01923(16) Uani 1.00 1 d . . . P(9) P 0.49274(7) 0.18565(4) 0.06852(5) 0.0425(2) Uani 1.00 1 d . . . F(1) F 0.5142(2) 0.13958(12) 0.11496(19) 0.0812(10) Uani 1.00 1 d . . . F(2) F 0.41287(19) 0.16412(14) 0.05459(18) 0.0808(10) Uani 1.00 1 d . . . F(3) F 0.46645(16) 0.21426(12) 0.13175(15) 0.0610(7) Uani 1.00 1 d . . . F(4) F 0.4705(2) 0.23513(16) 0.0268(2) 0.1033(15) Uani 1.00 1 d . . . F(5) F 0.57298(17) 0.20731(12) 0.08365(15) 0.0640(8) Uani 1.00 1 d . . . F(6) F 0.5156(2) 0.15888(19) 0.0063(2) 0.1190(18) Uani 1.00 1 d . . . N(1) N 0.78782(17) -0.04643(12) 0.35788(15) 0.0305(6) Uani 1.00 1 d . . . N(2) N 0.25798(19) 0.42313(14) 0.33582(17) 0.0391(8) Uani 1.00 1 d . . . C(1) C 0.7519(2) -0.01429(14) 0.33548(19) 0.0303(7) Uani 1.00 1 d . . . C(2) C 0.2935(2) 0.38945(15) 0.32409(18) 0.0314(7) Uani 1.00 1 d . . . C(3) C 0.50424(18) 0.05094(13) 0.23923(16) 0.0240(6) Uani 1.00 1 d . . . C(4) C 0.41382(17) 0.13240(12) 0.25550(15) 0.0199(6) Uani 1.00 1 d . . . C(5) C 0.31822(17) 0.21312(12) 0.23142(16) 0.0218(6) Uani 1.00 1 d . . . C(6) C 0.68590(19) 0.15372(13) 0.21872(17) 0.0247(6) Uani 1.00 1 d . . . C(7) C 0.60707(18) 0.23875(12) 0.24335(16) 0.0220(6) Uani 1.00 1 d . . . C(8) C 0.51211(18) 0.31798(12) 0.22051(16) 0.0232(6) Uani 1.00 1 d . . . C(11) C 0.8301(2) -0.08569(15) 0.38632(18) 0.0318(8) Uani 1.00 1 d . . . C(12) C 0.8959(2) -0.07321(17) 0.42144(19) 0.0387(9) Uani 1.00 1 d . . . C(13) C 0.9368(2) -0.1129(2) 0.4494(2) 0.0523(12) Uani 1.00 1 d . . . C(14) C 0.9133(3) -0.1617(2) 0.4421(2) 0.0583(15) Uani 1.00 1 d . . . C(15) C 0.8482(2) -0.17283(17) 0.4074(2) 0.0501(12) Uani 1.00 1 d . . . C(16) C 0.8046(2) -0.13481(15) 0.3779(2) 0.0377(9) Uani 1.00 1 d . . . C(17) C 0.9211(2) -0.0194(2) 0.4293(2) 0.0520(11) Uani 1.00 1 d . . . C(18) C 0.7336(2) -0.14586(17) 0.3401(2) 0.0479(10) Uani 1.00 1 d . . . C(21) C 0.2150(2) 0.4636(2) 0.3531(2) 0.0556(14) Uani 1.00 1 d . . . C(22) C 0.2410(4) 0.5109(2) 0.3466(2) 0.0711(17) Uani 1.00 1 d . . . C(23) C 0.1955(6) 0.5514(3) 0.3683(3) 0.112(3) Uani 1.00 1 d . . . C(24) C 0.1282(5) 0.5351(4) 0.3916(3) 0.103(3) Uani 1.00 1 d . . . C(25) C 0.1051(5) 0.4905(4) 0.3941(3) 0.110(3) Uani 1.00 1 d . . . C(26) C 0.1467(3) 0.4502(3) 0.3768(2) 0.075(2) Uani 1.00 1 d . . . C(27) C 0.3112(5) 0.5207(2) 0.3189(4) 0.112(3) Uani 1.00 1 d . . . C(28) C 0.1217(4) 0.3988(4) 0.3815(3) 0.107(3) Uani 1.00 1 d . . . C(101) C 0.58583(19) -0.02280(13) 0.18006(17) 0.0268(7) Uani 1.00 1 d . . . C(102) C 0.5861(2) 0.00731(15) 0.1243(2) 0.0358(8) Uani 1.00 1 d . . . C(103) C 0.5910(2) -0.01412(19) 0.0631(2) 0.0479(10) Uani 1.00 1 d . . . C(104) C 0.5961(2) -0.0661(2) 0.0568(2) 0.0527(12) Uani 1.00 1 d . . . C(105) C 0.5975(2) -0.09590(17) 0.1118(2) 0.0487(11) Uani 1.00 1 d . . . C(106) C 0.5932(2) -0.07475(15) 0.1734(2) 0.0364(8) Uani 1.00 1 d . . . C(107) C 0.53999(19) -0.04315(13) 0.30708(18) 0.0264(7) Uani 1.00 1 d . . . C(108) C 0.4796(2) -0.07068(16) 0.2817(2) 0.0392(9) Uani 1.00 1 d . . . C(109) C 0.4547(2) -0.11075(18) 0.3167(2) 0.0480(10) Uani 1.00 1 d . . . C(110) C 0.4885(2) -0.12372(17) 0.3770(2) 0.0463(10) Uani 1.00 1 d . . . C(111) C 0.5472(2) -0.09639(16) 0.4032(2) 0.0413(9) Uani 1.00 1 d . . . C(112) C 0.5736(2) -0.05617(14) 0.36792(19) 0.0322(8) Uani 1.00 1 d . . . C(113) C 0.43111(18) 0.05657(12) 0.35581(16) 0.0215(6) Uani 1.00 1 d . . . C(114) C 0.3680(2) 0.03217(14) 0.33092(18) 0.0305(7) Uani 1.00 1 d . . . C(115) C 0.3288(2) 0.00225(15) 0.3709(2) 0.0364(8) Uani 1.00 1 d . . . C(116) C 0.3527(2) -0.00371(14) 0.4362(2) 0.0344(8) Uani 1.00 1 d . . . C(117) C 0.4158(2) 0.01942(15) 0.46131(19) 0.0362(8) Uani 1.00 1 d . . . C(118) C 0.4550(2) 0.04985(14) 0.42113(18) 0.0302(7) Uani 1.00 1 d . . . C(119) C 0.31289(18) 0.15710(13) 0.35081(17) 0.0247(6) Uani 1.00 1 d . . . C(120) C 0.2485(2) 0.13450(15) 0.3256(2) 0.0350(8) Uani 1.00 1 d . . . C(121) C 0.2003(2) 0.11387(17) 0.3671(2) 0.0453(10) Uani 1.00 1 d . . . C(122) C 0.2171(2) 0.11528(19) 0.4341(2) 0.0518(12) Uani 1.00 1 d . . . C(123) C 0.2808(2) 0.1369(2) 0.4589(2) 0.0554(12) Uani 1.00 1 d . . . C(124) C 0.3287(2) 0.15806(17) 0.4182(2) 0.0398(9) Uani 1.00 1 d . . . C(125) C 0.19939(19) 0.26116(13) 0.29663(18) 0.0262(7) Uani 1.00 1 d . . . C(126) C 0.1299(2) 0.25360(16) 0.2671(2) 0.0385(9) Uani 1.00 1 d . . . C(127) C 0.0714(2) 0.2476(2) 0.3052(2) 0.0544(12) Uani 1.00 1 d . . . C(128) C 0.0825(2) 0.2484(2) 0.3725(2) 0.0547(12) Uani 1.00 1 d . . . C(129) C 0.1513(2) 0.25556(19) 0.4025(2) 0.0508(11) Uani 1.00 1 d . . . C(130) C 0.2097(2) 0.26235(16) 0.3648(2) 0.0360(8) Uani 1.00 1 d . . . C(131) C 0.23706(18) 0.29381(13) 0.17039(16) 0.0240(6) Uani 1.00 1 d . . . C(132) C 0.22666(19) 0.34513(13) 0.16029(17) 0.0274(7) Uani 1.00 1 d . . . C(133) C 0.1941(2) 0.36312(14) 0.10150(19) 0.0327(8) Uani 1.00 1 d . . . C(134) C 0.1716(2) 0.33042(15) 0.05192(18) 0.0331(8) Uani 1.00 1 d . . . C(135) C 0.1819(2) 0.27973(16) 0.0612(2) 0.0447(10) Uani 1.00 1 d . . . C(136) C 0.2148(2) 0.26122(15) 0.1201(2) 0.0408(9) Uani 1.00 1 d . . . C(201) C 0.7469(2) 0.07129(14) 0.15391(18) 0.0308(7) Uani 1.00 1 d . . . C(202) C 0.7341(3) 0.1000(2) 0.0977(2) 0.0623(15) Uani 1.00 1 d . . . C(203) C 0.7464(4) 0.0800(2) 0.0371(2) 0.080(2) Uani 1.00 1 d . . . C(204) C 0.7721(3) 0.0317(2) 0.0321(2) 0.0630(15) Uani 1.00 1 d . . . C(205) C 0.7839(2) 0.00310(18) 0.0868(2) 0.0504(11) Uani 1.00 1 d . . . C(206) C 0.7706(2) 0.02248(16) 0.1473(2) 0.0380(9) Uani 1.00 1 d . . . C(207) C 0.82696(19) 0.11241(13) 0.26678(17) 0.0246(6) Uani 1.00 1 d . . . C(208) C 0.8455(2) 0.10925(14) 0.33412(18) 0.0302(7) Uani 1.00 1 d . . . C(209) C 0.9154(2) 0.12075(17) 0.3597(2) 0.0404(9) Uani 1.00 1 d . . . C(210) C 0.9678(2) 0.13488(17) 0.3187(2) 0.0439(10) Uani 1.00 1 d . . . C(211) C 0.9496(2) 0.13822(17) 0.2523(2) 0.0441(10) Uani 1.00 1 d . . . C(212) C 0.8795(2) 0.12742(15) 0.2261(2) 0.0351(8) Uani 1.00 1 d . . . C(213) C 0.73429(18) 0.21539(12) 0.32841(17) 0.0233(6) Uani 1.00 1 d . . . C(214) C 0.7435(2) 0.21632(14) 0.39637(18) 0.0306(7) Uani 1.00 1 d . . . C(215) C 0.8053(2) 0.23908(15) 0.4276(2) 0.0403(9) Uani 1.00 1 d . . . C(216) C 0.8571(2) 0.25976(16) 0.3919(2) 0.0420(10) Uani 1.00 1 d . . . C(217) C 0.8487(2) 0.25853(16) 0.3243(2) 0.0410(9) Uani 1.00 1 d . . . C(218) C 0.7872(2) 0.23699(15) 0.2925(2) 0.0328(8) Uani 1.00 1 d . . . C(219) C 0.61099(18) 0.31685(12) 0.33888(17) 0.0235(6) Uani 1.00 1 d . . . C(220) C 0.6145(2) 0.31194(14) 0.40651(18) 0.0300(7) Uani 1.00 1 d . . . C(221) C 0.6674(2) 0.33746(15) 0.4457(2) 0.0386(9) Uani 1.00 1 d . . . C(222) C 0.7172(2) 0.36743(17) 0.4174(2) 0.0440(10) Uani 1.00 1 d . . . C(223) C 0.7132(2) 0.37341(18) 0.3508(2) 0.0475(11) Uani 1.00 1 d . . . C(224) C 0.6602(2) 0.34821(16) 0.3109(2) 0.0378(9) Uani 1.00 1 d . . . C(225) C 0.48700(18) 0.41661(12) 0.27421(17) 0.0240(6) Uani 1.00 1 d . . . C(226) C 0.4775(2) 0.42958(15) 0.33889(19) 0.0335(8) Uani 1.00 1 d . . . C(227) C 0.5091(2) 0.47324(18) 0.3656(2) 0.0462(10) Uani 1.00 1 d . . . C(228) C 0.5487(2) 0.50450(17) 0.3283(2) 0.0451(10) Uani 1.00 1 d . . . C(229) C 0.5593(2) 0.49144(16) 0.2643(2) 0.0421(9) Uani 1.00 1 d . . . C(230) C 0.5299(2) 0.44754(15) 0.23771(19) 0.0337(8) Uani 1.00 1 d . . . C(231) C 0.40526(18) 0.38345(12) 0.15723(16) 0.0224(6) Uani 1.00 1 d . . . C(232) C 0.3812(2) 0.43292(14) 0.14796(19) 0.0309(7) Uani 1.00 1 d . . . C(233) C 0.3493(2) 0.44873(16) 0.0873(2) 0.0385(9) Uani 1.00 1 d . . . C(234) C 0.3400(2) 0.41523(16) 0.0355(2) 0.0384(9) Uani 1.00 1 d . . . C(235) C 0.3634(2) 0.36579(16) 0.04414(19) 0.0358(8) Uani 1.00 1 d . . . C(236) C 0.3957(2) 0.35025(13) 0.10463(18) 0.0276(7) Uani 1.00 1 d . . . C(301) C -0.0143(4) 0.8830(3) 0.9865(4) 0.118(3) Uani 1.00 1 d D . . C(302) C 0.1015(5) 0.7483(4) 0.9415(4) 0.147(4) Uani 1.00 1 d D . . H(1) H 0.5160 0.0698 0.2019 0.029 Uiso 1.00 1 c R . . H(2) H 0.4615 0.0317 0.2275 0.029 Uiso 1.00 1 c R . . H(3) H 0.4345 0.1450 0.2176 0.025 Uiso 1.00 1 c R . . H(4) H 0.3745 0.1107 0.2420 0.025 Uiso 1.00 1 c R . . H(5) H 0.3458 0.2172 0.1945 0.027 Uiso 1.00 1 c R . . H(6) H 0.2795 0.1899 0.2201 0.027 Uiso 1.00 1 c R . . H(7) H 0.7180 0.1760 0.1988 0.031 Uiso 1.00 1 c R . . H(8) H 0.6454 0.1467 0.1880 0.031 Uiso 1.00 1 c R . . H(9) H 0.6441 0.2601 0.2286 0.027 Uiso 1.00 1 c R . . H(10) H 0.5793 0.2253 0.2061 0.027 Uiso 1.00 1 c R . . H(11) H 0.5515 0.3371 0.2067 0.029 Uiso 1.00 1 c R . . H(12) H 0.4936 0.2968 0.1854 0.029 Uiso 1.00 1 c R . . H(13) H 0.9272 -0.0106 0.4743 0.064 Uiso 1.00 1 c R . . H(14) H 0.9666 -0.0153 0.4106 0.064 Uiso 1.00 1 c R . . H(15) H 0.8864 0.0025 0.4072 0.064 Uiso 1.00 1 c R . . H(16) H 0.6948 -0.1294 0.3595 0.058 Uiso 1.00 1 c R . . H(17) H 0.7343 -0.1337 0.2958 0.058 Uiso 1.00 1 c R . . H(18) H 0.7247 -0.1810 0.3386 0.058 Uiso 1.00 1 c R . . H(19) H 0.3534 0.5043 0.3434 0.120 Uiso 1.00 1 c R . . H(20) H 0.3138 0.5076 0.2737 0.120 Uiso 1.00 1 c R . . H(21) H 0.3254 0.5558 0.3160 0.120 Uiso 1.00 1 c R . . H(22) H 0.1132 0.3877 0.4259 0.124 Uiso 1.00 1 c R . . H(23) H 0.0772 0.3908 0.3548 0.124 Uiso 1.00 1 c R . . H(24) H 0.1575 0.3737 0.3674 0.124 Uiso 1.00 1 c R . . H(25) H 0.9821 -0.1060 0.4741 0.064 Uiso 1.00 1 c R . . H(26) H 0.9433 -0.1881 0.4611 0.071 Uiso 1.00 1 c R . . H(27) H 0.8325 -0.2073 0.4038 0.061 Uiso 1.00 1 c R . . H(28) H 0.2179 0.5857 0.3638 0.178 Uiso 1.00 1 c R . . H(29) H 0.1040 0.5676 0.4047 0.219 Uiso 1.00 1 c R . . H(30) H 0.0597 0.4873 0.4096 0.172 Uiso 1.00 1 c R . . H(31) H 0.5827 0.0430 0.1285 0.044 Uiso 1.00 1 c R . . H(32) H 0.5908 0.0070 0.0251 0.060 Uiso 1.00 1 c R . . H(33) H 0.5987 -0.0806 0.0144 0.063 Uiso 1.00 1 c R . . H(34) H 0.6010 -0.1316 0.1070 0.060 Uiso 1.00 1 c R . . H(35) H 0.5953 -0.0959 0.2114 0.045 Uiso 1.00 1 c R . . H(36) H 0.4552 -0.0614 0.2404 0.048 Uiso 1.00 1 c R . . H(37) H 0.4139 -0.1301 0.2985 0.059 Uiso 1.00 1 c R . . H(38) H 0.4710 -0.1518 0.4004 0.057 Uiso 1.00 1 c R . . H(39) H 0.5697 -0.1049 0.4460 0.050 Uiso 1.00 1 c R . . H(40) H 0.6155 -0.0374 0.3857 0.039 Uiso 1.00 1 c R . . H(41) H 0.3517 0.0362 0.2858 0.037 Uiso 1.00 1 c R . . H(42) H 0.2852 -0.0142 0.3530 0.045 Uiso 1.00 1 c R . . H(43) H 0.3254 -0.0240 0.4640 0.042 Uiso 1.00 1 c R . . H(44) H 0.4327 0.0148 0.5067 0.043 Uiso 1.00 1 c R . . H(45) H 0.4985 0.0663 0.4386 0.037 Uiso 1.00 1 c R . . H(46) H 0.2372 0.1336 0.2789 0.043 Uiso 1.00 1 c R . . H(47) H 0.1560 0.0983 0.3487 0.055 Uiso 1.00 1 c R . . H(48) H 0.1846 0.1010 0.4632 0.064 Uiso 1.00 1 c R . . H(49) H 0.2924 0.1377 0.5057 0.067 Uiso 1.00 1 c R . . H(50) H 0.3727 0.1741 0.4364 0.049 Uiso 1.00 1 c R . . H(51) H 0.1226 0.2527 0.2201 0.047 Uiso 1.00 1 c R . . H(52) H 0.0230 0.2427 0.2841 0.066 Uiso 1.00 1 c R . . H(53) H 0.0421 0.2440 0.3985 0.066 Uiso 1.00 1 c R . . H(54) H 0.1591 0.2562 0.4498 0.062 Uiso 1.00 1 c R . . H(55) H 0.2576 0.2678 0.3853 0.044 Uiso 1.00 1 c R . . H(56) H 0.2421 0.3682 0.1945 0.034 Uiso 1.00 1 c R . . H(57) H 0.1875 0.3986 0.0954 0.040 Uiso 1.00 1 c R . . H(58) H 0.1494 0.3427 0.0112 0.040 Uiso 1.00 1 c R . . H(59) H 0.1667 0.2566 0.0269 0.053 Uiso 1.00 1 c R . . H(60) H 0.2224 0.2258 0.1255 0.050 Uiso 1.00 1 c R . . H(61) H 0.7176 0.1341 0.1011 0.078 Uiso 1.00 1 c R . . H(62) H 0.7362 0.0999 -0.0014 0.096 Uiso 1.00 1 c R . . H(63) H 0.7820 0.0188 -0.0103 0.075 Uiso 1.00 1 c R . . H(64) H 0.8015 -0.0307 0.0835 0.061 Uiso 1.00 1 c R . . H(65) H 0.7776 0.0014 0.1855 0.048 Uiso 1.00 1 c R . . H(66) H 0.8099 0.0992 0.3627 0.037 Uiso 1.00 1 c R . . H(67) H 0.9277 0.1183 0.4060 0.049 Uiso 1.00 1 c R . . H(68) H 1.0166 0.1420 0.3361 0.053 Uiso 1.00 1 c R . . H(69) H 0.9854 0.1489 0.2240 0.055 Uiso 1.00 1 c R . . H(70) H 0.8671 0.1301 0.1797 0.043 Uiso 1.00 1 c R . . H(71) H 0.7075 0.2012 0.4215 0.038 Uiso 1.00 1 c R . . H(72) H 0.8113 0.2406 0.4748 0.049 Uiso 1.00 1 c R . . H(73) H 0.8995 0.2752 0.4138 0.050 Uiso 1.00 1 c R . . H(74) H 0.8854 0.2728 0.2993 0.050 Uiso 1.00 1 c R . . H(75) H 0.7810 0.2365 0.2455 0.041 Uiso 1.00 1 c R . . H(76) H 0.5801 0.2910 0.4264 0.037 Uiso 1.00 1 c R . . H(77) H 0.6698 0.3340 0.4924 0.047 Uiso 1.00 1 c R . . H(78) H 0.7541 0.3845 0.4447 0.053 Uiso 1.00 1 c R . . H(79) H 0.7476 0.3946 0.3312 0.058 Uiso 1.00 1 c R . . H(80) H 0.6565 0.3529 0.2643 0.046 Uiso 1.00 1 c R . . H(81) H 0.4490 0.4083 0.3649 0.041 Uiso 1.00 1 c R . . H(82) H 0.5030 0.4816 0.4107 0.057 Uiso 1.00 1 c R . . H(83) H 0.5695 0.5351 0.3469 0.054 Uiso 1.00 1 c R . . H(84) H 0.5870 0.5133 0.2383 0.052 Uiso 1.00 1 c R . . H(85) H 0.5383 0.4382 0.1936 0.041 Uiso 1.00 1 c R . . H(86) H 0.3862 0.4562 0.1839 0.038 Uiso 1.00 1 c R . . H(87) H 0.3336 0.4829 0.0817 0.047 Uiso 1.00 1 c R . . H(88) H 0.3180 0.4262 -0.0061 0.046 Uiso 1.00 1 c R . . H(89) H 0.3568 0.3422 0.0087 0.044 Uiso 1.00 1 c R . . H(90) H 0.4120 0.3162 0.1097 0.034 Uiso 1.00 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0242(2) 0.0214(2) 0.0278(2) 0.00085(16) -0.00429(16) 0.00097(16) Cu(2) 0.0231(2) 0.0229(2) 0.0241(2) -0.00290(16) -0.00240(16) 0.00098(16) Cu(3) 0.0228(2) 0.0235(2) 0.0232(2) -0.00311(16) -0.00080(16) 0.00002(16) Cu(4) 0.0210(2) 0.0224(2) 0.0232(2) -0.00118(16) 0.00226(15) -0.00105(15) Cl(1) 0.0294(4) 0.0260(4) 0.0253(4) 0.0031(3) -0.0049(3) 0.0015(3) Cl(2) 0.0286(4) 0.0273(4) 0.0241(3) 0.0026(3) -0.0040(3) -0.0003(3) Cl(3) 0.0299(4) 0.0296(4) 0.0248(4) 0.0031(3) 0.0006(3) -0.0019(3) Cl(11) 0.1150(16) 0.1204(17) 0.1092(16) 0.0016(13) 0.0198(13) 0.0390(13) Cl(12) 0.145(3) 0.305(8) 0.106(3) -0.024(4) 0.013(2) 0.042(4) Cl(13) 0.126(7) 0.140(9) 0.130(8) -0.003(5) 0.009(5) 0.068(7) Cl(14) 0.178(2) 0.137(2) 0.151(2) 0.008(2) 0.042(2) -0.0237(19) Cl(15) 0.31(2) 0.124(8) 0.146(13) -0.053(13) -0.101(17) 0.052(8) Cl(16) 0.148(7) 0.106(4) 0.100(3) 0.001(3) 0.009(4) 0.001(3) P(1) 0.0226(4) 0.0196(4) 0.0241(4) 0.0008(3) -0.0021(3) -0.0019(3) P(2) 0.0197(3) 0.0178(3) 0.0193(3) 0.0001(3) -0.0012(3) 0.0006(3) P(3) 0.0187(3) 0.0186(3) 0.0197(3) -0.0001(3) 0.0001(3) 0.0011(3) P(4) 0.0191(3) 0.0200(3) 0.0214(4) 0.0008(3) -0.0004(3) 0.0015(3) P(5) 0.0241(4) 0.0203(4) 0.0240(4) 0.0043(3) -0.0015(3) -0.0002(3) P(6) 0.0198(4) 0.0184(3) 0.0219(4) 0.0011(3) -0.0009(3) -0.0002(3) P(7) 0.0192(3) 0.0183(3) 0.0209(3) 0.0007(3) 0.0007(3) -0.0005(3) P(8) 0.0198(3) 0.0176(3) 0.0204(3) 0.0010(3) 0.0022(3) 0.0002(3) P(9) 0.0555(7) 0.0387(5) 0.0325(5) -0.0171(5) -0.0017(4) -0.0010(4) F(1) 0.088(2) 0.059(2) 0.100(2) 0.0179(17) 0.034(2) 0.0375(18) F(2) 0.075(2) 0.076(2) 0.090(2) -0.0349(18) -0.0041(18) -0.0276(19) F(3) 0.0600(17) 0.0609(18) 0.0613(18) 0.0020(14) 0.0000(14) -0.0250(14) F(4) 0.119(3) 0.093(2) 0.088(2) -0.036(2) -0.047(2) 0.049(2) F(5) 0.0647(18) 0.071(2) 0.0551(17) -0.0259(15) -0.0004(14) -0.0026(15) F(6) 0.132(3) 0.142(3) 0.091(2) -0.071(3) 0.053(2) -0.076(2) N(1) 0.0308(16) 0.0302(16) 0.0306(15) 0.0074(13) 0.0039(12) 0.0041(12) N(2) 0.0374(18) 0.044(2) 0.0344(17) 0.0150(15) -0.0035(14) -0.0083(15) C(1) 0.0283(18) 0.0285(18) 0.0338(19) 0.0027(14) 0.0010(14) 0.0001(15) C(2) 0.0296(19) 0.0334(19) 0.0310(19) 0.0037(15) 0.0018(14) -0.0029(15) C(3) 0.0239(16) 0.0239(16) 0.0235(16) 0.0009(13) -0.0023(12) -0.0013(12) C(4) 0.0191(15) 0.0214(15) 0.0189(14) 0.0001(12) -0.0006(11) 0.0018(11) C(5) 0.0197(15) 0.0227(15) 0.0226(15) -0.0006(12) -0.0008(12) 0.0005(12) C(6) 0.0248(16) 0.0239(16) 0.0248(16) 0.0040(13) -0.0023(13) -0.0013(12) C(7) 0.0226(16) 0.0212(15) 0.0220(15) 0.0021(12) 0.0005(12) 0.0006(12) C(8) 0.0242(16) 0.0208(15) 0.0249(16) 0.0035(12) 0.0027(12) 0.0001(12) C(11) 0.0332(19) 0.0346(19) 0.0286(18) 0.0164(15) 0.0091(15) 0.0077(15) C(12) 0.038(2) 0.049(2) 0.0297(19) 0.0187(18) 0.0073(16) 0.0019(17) C(13) 0.049(2) 0.070(3) 0.038(2) 0.037(2) 0.0083(19) 0.011(2) C(14) 0.063(3) 0.066(3) 0.049(2) 0.049(2) 0.024(2) 0.026(2) C(15) 0.064(3) 0.041(2) 0.050(2) 0.029(2) 0.034(2) 0.019(2) C(16) 0.042(2) 0.036(2) 0.037(2) 0.0110(17) 0.0182(17) 0.0066(16) C(17) 0.045(2) 0.064(3) 0.047(2) 0.011(2) -0.001(2) -0.015(2) C(18) 0.053(2) 0.040(2) 0.053(2) 0.002(2) 0.020(2) -0.001(2) C(21) 0.060(3) 0.067(3) 0.038(2) 0.048(2) -0.010(2) -0.013(2) C(22) 0.093(4) 0.059(3) 0.055(3) 0.029(3) -0.026(3) -0.009(2) C(23) 0.173(9) 0.084(5) 0.066(4) 0.048(5) -0.061(5) -0.011(3) C(24) 0.116(7) 0.135(7) 0.052(3) 0.070(6) -0.031(4) -0.029(4) C(25) 0.104(6) 0.170(9) 0.053(3) 0.077(6) -0.015(3) -0.017(5) C(26) 0.057(3) 0.129(6) 0.037(2) 0.045(3) -0.008(2) -0.009(3) C(27) 0.139(7) 0.065(4) 0.119(6) -0.011(4) -0.065(5) 0.013(4) C(28) 0.063(4) 0.179(9) 0.078(4) 0.023(5) -0.002(3) 0.035(5) C(101) 0.0226(16) 0.0277(17) 0.0298(18) 0.0002(13) -0.0005(13) -0.0085(14) C(102) 0.037(2) 0.036(2) 0.035(2) 0.0017(16) 0.0044(16) -0.0072(16) C(103) 0.054(2) 0.055(2) 0.035(2) 0.004(2) 0.0074(19) -0.0122(19) C(104) 0.052(2) 0.061(3) 0.046(2) -0.000(2) 0.009(2) -0.032(2) C(105) 0.047(2) 0.039(2) 0.062(3) -0.0001(19) 0.014(2) -0.026(2) C(106) 0.034(2) 0.0310(19) 0.044(2) 0.0019(16) 0.0049(17) -0.0096(16) C(107) 0.0267(17) 0.0214(16) 0.0307(18) 0.0003(13) 0.0007(13) -0.0005(13) C(108) 0.034(2) 0.037(2) 0.046(2) -0.0064(17) -0.0011(17) 0.0005(17) C(109) 0.043(2) 0.041(2) 0.060(2) -0.0124(19) 0.003(2) 0.003(2) C(110) 0.046(2) 0.036(2) 0.059(2) -0.0015(19) 0.018(2) 0.015(2) C(111) 0.042(2) 0.039(2) 0.044(2) 0.0066(18) 0.0087(18) 0.0114(18) C(112) 0.0333(19) 0.0285(18) 0.0343(19) 0.0013(15) 0.0006(15) 0.0040(15) C(113) 0.0238(16) 0.0182(14) 0.0223(15) 0.0016(12) 0.0000(12) 0.0004(12) C(114) 0.0319(19) 0.0305(18) 0.0280(18) -0.0077(15) -0.0032(14) 0.0037(14) C(115) 0.035(2) 0.033(2) 0.040(2) -0.0089(16) -0.0019(16) 0.0057(16) C(116) 0.039(2) 0.0296(19) 0.036(2) -0.0041(16) 0.0112(16) 0.0060(15) C(117) 0.046(2) 0.035(2) 0.0280(19) -0.0040(17) 0.0049(16) 0.0038(15) C(118) 0.0336(19) 0.0305(18) 0.0258(17) -0.0038(15) -0.0015(14) 0.0011(14) C(119) 0.0246(16) 0.0233(16) 0.0270(17) 0.0049(13) 0.0082(13) 0.0019(13) C(120) 0.033(2) 0.035(2) 0.038(2) -0.0071(16) 0.0081(16) 0.0021(16) C(121) 0.040(2) 0.040(2) 0.058(2) -0.0081(18) 0.018(2) 0.004(2) C(122) 0.048(2) 0.055(2) 0.057(2) 0.004(2) 0.030(2) 0.021(2) C(123) 0.057(3) 0.072(3) 0.040(2) 0.003(2) 0.017(2) 0.014(2) C(124) 0.035(2) 0.051(2) 0.034(2) 0.0044(18) 0.0083(16) 0.0043(18) C(125) 0.0232(16) 0.0248(16) 0.0311(18) -0.0006(13) 0.0047(13) 0.0029(13) C(126) 0.0295(19) 0.039(2) 0.047(2) -0.0035(16) 0.0029(17) 0.0026(18) C(127) 0.034(2) 0.059(3) 0.072(3) -0.007(2) 0.011(2) 0.003(2) C(128) 0.044(2) 0.057(2) 0.068(3) -0.006(2) 0.029(2) 0.005(2) C(129) 0.050(2) 0.056(2) 0.050(2) -0.006(2) 0.021(2) 0.003(2) C(130) 0.032(2) 0.041(2) 0.036(2) -0.0026(16) 0.0093(16) 0.0020(17) C(131) 0.0218(16) 0.0253(16) 0.0246(16) 0.0017(12) -0.0002(12) 0.0011(13) C(132) 0.0274(17) 0.0258(17) 0.0278(17) 0.0031(13) -0.0042(14) 0.0013(13) C(133) 0.0331(19) 0.0297(18) 0.0346(19) 0.0049(15) -0.0018(15) 0.0080(15) C(134) 0.0331(19) 0.037(2) 0.0277(18) 0.0039(16) -0.0049(14) 0.0055(15) C(135) 0.058(2) 0.038(2) 0.035(2) 0.0059(19) -0.0199(19) -0.0046(17) C(136) 0.053(2) 0.0283(19) 0.037(2) 0.0067(17) -0.0152(18) -0.0027(16) C(201) 0.0328(19) 0.0291(18) 0.0298(18) 0.0055(14) -0.0018(14) -0.0040(14) C(202) 0.095(4) 0.051(2) 0.041(2) 0.034(2) 0.000(2) -0.001(2) C(203) 0.121(5) 0.073(4) 0.043(2) 0.041(3) -0.002(3) -0.002(2) C(204) 0.080(3) 0.065(3) 0.043(2) 0.027(2) -0.003(2) -0.022(2) C(205) 0.055(2) 0.044(2) 0.052(2) 0.010(2) 0.006(2) -0.020(2) C(206) 0.040(2) 0.035(2) 0.040(2) 0.0064(17) 0.0052(17) -0.0039(16) C(207) 0.0246(16) 0.0214(15) 0.0277(17) 0.0059(13) 0.0014(13) 0.0006(12) C(208) 0.0278(18) 0.0320(18) 0.0305(18) -0.0002(14) 0.0009(14) 0.0007(14) C(209) 0.035(2) 0.042(2) 0.042(2) -0.0009(17) -0.0059(17) 0.0020(18) C(210) 0.031(2) 0.044(2) 0.056(2) -0.0043(18) -0.0015(18) 0.000(2) C(211) 0.035(2) 0.046(2) 0.053(2) -0.0053(18) 0.0156(19) 0.002(2) C(212) 0.036(2) 0.034(2) 0.035(2) 0.0015(16) 0.0065(16) 0.0035(16) C(213) 0.0214(15) 0.0200(15) 0.0279(17) 0.0038(12) -0.0022(12) -0.0014(12) C(214) 0.0320(19) 0.0280(18) 0.0305(18) 0.0004(14) -0.0059(14) -0.0045(14) C(215) 0.042(2) 0.034(2) 0.041(2) 0.0024(17) -0.0185(18) -0.0059(17) C(216) 0.034(2) 0.032(2) 0.057(2) -0.0011(16) -0.0161(19) -0.0069(18) C(217) 0.030(2) 0.038(2) 0.055(2) -0.0063(16) 0.0006(18) 0.0004(19) C(218) 0.0298(19) 0.0330(19) 0.036(2) -0.0030(15) 0.0030(15) -0.0013(15) C(219) 0.0221(16) 0.0213(15) 0.0267(16) 0.0018(12) 0.0003(12) -0.0038(12) C(220) 0.0319(19) 0.0265(17) 0.0307(18) -0.0020(14) -0.0023(14) -0.0032(14) C(221) 0.045(2) 0.032(2) 0.037(2) -0.0046(17) -0.0088(17) -0.0066(16) C(222) 0.040(2) 0.041(2) 0.049(2) -0.0084(18) -0.0080(19) -0.0143(19) C(223) 0.042(2) 0.053(2) 0.049(2) -0.023(2) 0.0077(19) -0.012(2) C(224) 0.037(2) 0.041(2) 0.036(2) -0.0162(17) 0.0075(16) -0.0063(17) C(225) 0.0232(16) 0.0208(15) 0.0280(17) 0.0004(12) 0.0017(13) -0.0020(12) C(226) 0.036(2) 0.033(2) 0.0317(19) -0.0081(15) 0.0065(15) -0.0051(15) C(227) 0.052(2) 0.046(2) 0.041(2) -0.015(2) 0.009(2) -0.0193(19) C(228) 0.048(2) 0.038(2) 0.050(2) -0.0124(19) 0.007(2) -0.0162(19) C(229) 0.044(2) 0.038(2) 0.045(2) -0.0183(18) 0.0093(19) -0.0043(18) C(230) 0.036(2) 0.0330(19) 0.0327(19) -0.0098(16) 0.0089(15) -0.0034(15) C(231) 0.0205(15) 0.0229(15) 0.0242(16) 0.0006(12) 0.0032(12) 0.0032(12) C(232) 0.0304(19) 0.0296(18) 0.0324(19) 0.0022(14) 0.0007(15) 0.0032(14) C(233) 0.036(2) 0.036(2) 0.043(2) 0.0071(17) 0.0003(17) 0.0149(17) C(234) 0.034(2) 0.045(2) 0.035(2) -0.0038(17) -0.0040(16) 0.0146(17) C(235) 0.036(2) 0.041(2) 0.0296(19) -0.0074(17) -0.0030(15) 0.0010(16) C(236) 0.0277(17) 0.0273(17) 0.0272(17) -0.0030(14) -0.0005(13) 0.0013(13) C(301) 0.092(5) 0.139(7) 0.119(6) -0.020(5) -0.024(4) 0.067(6) C(302) 0.135(8) 0.188(11) 0.111(7) 0.020(8) -0.021(6) 0.003(7) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cu(1) Cl(1) 2.3930(9) yes . . Cu(1) P(1) 2.2616(9) yes . . Cu(1) P(5) 2.2714(9) yes . . Cu(1) C(1) 1.933(3) yes . . Cu(2) Cl(1) 2.4247(9) yes . . Cu(2) Cl(2) 2.4008(9) yes . . Cu(2) P(2) 2.2574(8) yes . . Cu(2) P(6) 2.2582(9) yes . . Cu(3) Cl(2) 2.3935(9) yes . . Cu(3) Cl(3) 2.4112(9) yes . . Cu(3) P(3) 2.2408(8) yes . . Cu(3) P(7) 2.2509(8) yes . . Cu(4) Cl(3) 2.3769(8) yes . . Cu(4) P(4) 2.2647(8) yes . . Cu(4) P(8) 2.2645(8) yes . . Cu(4) C(2) 1.926(3) yes . . Cl(11) C(301) 1.747(8) yes . . Cl(12) C(301) 1.720(9) yes . . Cl(13) C(301) 1.869(13) yes . . Cl(14) C(302) 1.791(11) yes . . Cl(15) C(302) 1.73(3) yes . . Cl(16) C(302) 1.653(12) yes . . P(1) C(3) 1.842(3) yes . . P(1) C(101) 1.832(3) yes . . P(1) C(107) 1.822(3) yes . . P(2) C(3) 1.836(3) yes . . P(2) C(4) 1.847(3) yes . . P(2) C(113) 1.825(3) yes . . P(3) C(4) 1.839(3) yes . . P(3) C(5) 1.841(3) yes . . P(3) C(119) 1.829(3) yes . . P(4) C(5) 1.839(3) yes . . P(4) C(125) 1.833(3) yes . . P(4) C(131) 1.820(3) yes . . P(5) C(6) 1.841(3) yes . . P(5) C(201) 1.829(3) yes . . P(5) C(207) 1.827(3) yes . . P(6) C(6) 1.838(3) yes . . P(6) C(7) 1.842(3) yes . . P(6) C(213) 1.830(3) yes . . P(7) C(7) 1.837(3) yes . . P(7) C(8) 1.842(3) yes . . P(7) C(219) 1.826(3) yes . . P(8) C(8) 1.835(3) yes . . P(8) C(225) 1.820(3) yes . . P(8) C(231) 1.834(3) yes . . P(9) F(1) 1.581(3) yes . . P(9) F(2) 1.585(3) yes . . P(9) F(3) 1.612(3) yes . . P(9) F(4) 1.604(4) yes . . P(9) F(5) 1.596(3) yes . . P(9) F(6) 1.549(4) yes . . N(1) C(1) 1.154(4) yes . . N(1) C(11) 1.401(4) yes . . N(2) C(2) 1.148(5) yes . . N(2) C(21) 1.401(6) yes . . C(11) C(12) 1.399(5) yes . . C(11) C(16) 1.395(5) yes . . C(12) C(13) 1.394(6) yes . . C(12) C(17) 1.509(6) yes . . C(13) C(14) 1.372(7) yes . . C(14) C(15) 1.377(7) yes . . C(15) C(16) 1.397(6) yes . . C(16) C(18) 1.494(6) yes . . C(21) C(22) 1.358(8) yes . . C(21) C(26) 1.433(8) yes . . C(22) C(23) 1.458(11) yes . . C(22) C(27) 1.482(12) yes . . C(23) C(24) 1.434(15) yes . . C(24) C(25) 1.263(16) yes . . C(25) C(26) 1.380(13) yes . . C(26) C(28) 1.450(14) yes . . C(101) C(102) 1.396(5) yes . . C(101) C(106) 1.396(5) yes . . C(102) C(103) 1.385(6) yes . . C(103) C(104) 1.392(7) yes . . C(104) C(105) 1.378(7) yes . . C(105) C(106) 1.388(6) yes . . C(107) C(108) 1.397(5) yes . . C(107) C(112) 1.389(5) yes . . C(108) C(109) 1.384(6) yes . . C(109) C(110) 1.380(6) yes . . C(110) C(111) 1.376(6) yes . . C(111) C(112) 1.401(5) yes . . C(113) C(114) 1.393(4) yes . . C(113) C(118) 1.385(4) yes . . C(114) C(115) 1.388(5) yes . . C(115) C(116) 1.382(5) yes . . C(116) C(117) 1.379(5) yes . . C(117) C(118) 1.398(5) yes . . C(119) C(120) 1.393(5) yes . . C(119) C(124) 1.387(5) yes . . C(120) C(121) 1.393(6) yes . . C(121) C(122) 1.382(6) yes . . C(122) C(123) 1.367(7) yes . . C(123) C(124) 1.384(6) yes . . C(125) C(126) 1.387(5) yes . . C(125) C(130) 1.394(5) yes . . C(126) C(127) 1.392(6) yes . . C(127) C(128) 1.376(8) yes . . C(128) C(129) 1.378(6) yes . . C(129) C(130) 1.390(6) yes . . C(131) C(132) 1.391(4) yes . . C(131) C(136) 1.383(5) yes . . C(132) C(133) 1.385(5) yes . . C(133) C(134) 1.375(5) yes . . C(134) C(135) 1.373(5) yes . . C(135) C(136) 1.393(5) yes . . C(201) C(202) 1.384(6) yes . . C(201) C(206) 1.380(5) yes . . C(202) C(203) 1.387(7) yes . . C(203) C(204) 1.376(8) yes . . C(204) C(205) 1.357(7) yes . . C(205) C(206) 1.382(6) yes . . C(207) C(208) 1.396(4) yes . . C(207) C(212) 1.390(5) yes . . C(208) C(209) 1.385(5) yes . . C(209) C(210) 1.385(6) yes . . C(210) C(211) 1.377(6) yes . . C(211) C(212) 1.390(5) yes . . C(213) C(214) 1.388(5) yes . . C(213) C(218) 1.395(5) yes . . C(214) C(215) 1.398(5) yes . . C(215) C(216) 1.368(6) yes . . C(216) C(217) 1.379(6) yes . . C(217) C(218) 1.385(5) yes . . C(219) C(220) 1.387(5) yes . . C(219) C(224) 1.391(5) yes . . C(220) C(221) 1.389(5) yes . . C(221) C(222) 1.380(6) yes . . C(222) C(223) 1.370(6) yes . . C(223) C(224) 1.394(6) yes . . C(225) C(226) 1.394(5) yes . . C(225) C(230) 1.401(5) yes . . C(226) C(227) 1.392(6) yes . . C(227) C(228) 1.380(6) yes . . C(228) C(229) 1.385(6) yes . . C(229) C(230) 1.380(5) yes . . C(231) C(232) 1.397(4) yes . . C(231) C(236) 1.393(4) yes . . C(232) C(233) 1.394(5) yes . . C(233) C(234) 1.385(5) yes . . C(234) C(235) 1.391(5) yes . . C(235) C(236) 1.392(5) yes . . C(3) H(1) 0.955 no . . C(3) H(2) 0.955 no . . C(4) H(3) 0.955 no . . C(4) H(4) 0.951 no . . C(5) H(5) 0.953 no . . C(5) H(6) 0.958 no . . C(6) H(7) 0.954 no . . C(6) H(8) 0.954 no . . C(7) H(9) 0.957 no . . C(7) H(10) 0.952 no . . C(8) H(11) 0.950 no . . C(8) H(12) 0.955 no . . C(13) H(25) 0.960 no . . C(14) H(26) 0.957 no . . C(15) H(27) 0.962 no . . C(17) H(13) 0.949 no . . C(17) H(14) 0.958 no . . C(17) H(15) 0.952 no . . C(18) H(16) 0.955 no . . C(18) H(17) 0.964 no . . C(18) H(18) 0.949 no . . C(23) H(28) 1.009 no . . C(24) H(29) 1.021 no . . C(25) H(30) 0.924 no . . C(27) H(19) 0.992 no . . C(27) H(20) 0.995 no . . C(27) H(21) 0.972 no . . C(28) H(22) 0.980 no . . C(28) H(23) 0.971 no . . C(28) H(24) 0.999 no . . C(102) H(31) 0.956 no . . C(103) H(32) 0.960 no . . C(104) H(33) 0.955 no . . C(105) H(34) 0.957 no . . C(106) H(35) 0.960 no . . C(108) H(36) 0.957 no . . C(109) H(37) 0.960 no . . C(110) H(38) 0.957 no . . C(111) H(39) 0.965 no . . C(112) H(40) 0.964 no . . C(114) H(41) 0.954 no . . C(115) H(42) 0.962 no . . C(116) H(43) 0.958 no . . C(117) H(44) 0.963 no . . C(118) H(45) 0.957 no . . C(120) H(46) 0.961 no . . C(121) H(47) 0.964 no . . C(122) H(48) 0.959 no . . C(123) H(49) 0.965 no . . C(124) H(50) 0.965 no . . C(126) H(51) 0.961 no . . C(127) H(52) 0.969 no . . C(128) H(53) 0.960 no . . C(129) H(54) 0.967 no . . C(130) H(55) 0.957 no . . C(132) H(56) 0.957 no . . C(133) H(57) 0.959 no . . C(134) H(58) 0.956 no . . C(135) H(59) 0.958 no . . C(136) H(60) 0.957 no . . C(202) H(61) 0.963 no . . C(203) H(62) 0.955 no . . C(204) H(63) 0.965 no . . C(205) H(64) 0.961 no . . C(206) H(65) 0.962 no . . C(208) H(66) 0.954 no . . C(209) H(67) 0.958 no . . C(210) H(68) 0.960 no . . C(211) H(69) 0.957 no . . C(212) H(70) 0.960 no . . C(214) H(71) 0.962 no . . C(215) H(72) 0.964 no . . C(216) H(73) 0.961 no . . C(217) H(74) 0.962 no . . C(218) H(75) 0.960 no . . C(220) H(76) 0.960 no . . C(221) H(77) 0.959 no . . C(222) H(78) 0.957 no . . C(223) H(79) 0.962 no . . C(224) H(80) 0.958 no . . C(226) H(81) 0.964 no . . C(227) H(82) 0.965 no . . C(228) H(83) 0.964 no . . C(229) H(84) 0.964 no . . C(230) H(85) 0.962 no . . C(232) H(86) 0.961 no . . C(233) H(87) 0.958 no . . C(234) H(88) 0.958 no . . C(235) H(89) 0.960 no . . C(236) H(90) 0.957 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Cu(1) P(1) 107.43(3) yes . . . Cl(1) Cu(1) P(5) 109.47(3) yes . . . Cl(1) Cu(1) C(1) 101.99(11) yes . . . P(1) Cu(1) P(5) 112.15(3) yes . . . P(1) Cu(1) C(1) 111.26(11) yes . . . P(5) Cu(1) C(1) 113.85(11) yes . . . Cl(1) Cu(2) Cl(2) 107.95(3) yes . . . Cl(1) Cu(2) P(2) 106.57(3) yes . . . Cl(1) Cu(2) P(6) 103.30(3) yes . . . Cl(2) Cu(2) P(2) 103.82(3) yes . . . Cl(2) Cu(2) P(6) 111.79(3) yes . . . P(2) Cu(2) P(6) 122.68(3) yes . . . Cl(2) Cu(3) Cl(3) 103.42(3) yes . . . Cl(2) Cu(3) P(3) 106.66(3) yes . . . Cl(2) Cu(3) P(7) 108.77(3) yes . . . Cl(3) Cu(3) P(3) 108.23(3) yes . . . Cl(3) Cu(3) P(7) 103.15(3) yes . . . P(3) Cu(3) P(7) 124.70(3) yes . . . Cl(3) Cu(4) P(4) 111.07(3) yes . . . Cl(3) Cu(4) P(8) 108.46(3) yes . . . Cl(3) Cu(4) C(2) 104.37(11) yes . . . P(4) Cu(4) P(8) 114.44(3) yes . . . P(4) Cu(4) C(2) 109.17(11) yes . . . P(8) Cu(4) C(2) 108.82(11) yes . . . Cu(1) Cl(1) Cu(2) 93.44(3) yes . . . Cu(2) Cl(2) Cu(3) 87.77(3) yes . . . Cu(3) Cl(3) Cu(4) 90.18(3) yes . . . Cu(1) P(1) C(3) 117.76(11) yes . . . Cu(1) P(1) C(101) 113.46(11) yes . . . Cu(1) P(1) C(107) 115.69(11) yes . . . C(3) P(1) C(101) 99.75(15) yes . . . C(3) P(1) C(107) 105.26(16) yes . . . C(101) P(1) C(107) 102.74(16) yes . . . Cu(2) P(2) C(3) 115.92(11) yes . . . Cu(2) P(2) C(4) 115.37(10) yes . . . Cu(2) P(2) C(113) 119.57(10) yes . . . C(3) P(2) C(4) 97.67(14) yes . . . C(3) P(2) C(113) 101.96(15) yes . . . C(4) P(2) C(113) 103.21(14) yes . . . Cu(3) P(3) C(4) 112.94(10) yes . . . Cu(3) P(3) C(5) 116.16(10) yes . . . Cu(3) P(3) C(119) 119.39(11) yes . . . C(4) P(3) C(5) 98.94(14) yes . . . C(4) P(3) C(119) 103.74(15) yes . . . C(5) P(3) C(119) 103.01(14) yes . . . Cu(4) P(4) C(5) 118.04(10) yes . . . Cu(4) P(4) C(125) 111.59(11) yes . . . Cu(4) P(4) C(131) 113.19(11) yes . . . C(5) P(4) C(125) 107.09(15) yes . . . C(5) P(4) C(131) 102.12(15) yes . . . C(125) P(4) C(131) 103.44(15) yes . . . Cu(1) P(5) C(6) 117.89(12) yes . . . Cu(1) P(5) C(201) 115.71(12) yes . . . Cu(1) P(5) C(207) 111.76(11) yes . . . C(6) P(5) C(201) 101.58(16) yes . . . C(6) P(5) C(207) 105.52(15) yes . . . C(201) P(5) C(207) 102.69(17) yes . . . Cu(2) P(6) C(6) 115.40(11) yes . . . Cu(2) P(6) C(7) 115.33(11) yes . . . Cu(2) P(6) C(213) 120.12(11) yes . . . C(6) P(6) C(7) 97.13(15) yes . . . C(6) P(6) C(213) 102.64(15) yes . . . C(7) P(6) C(213) 102.94(14) yes . . . Cu(3) P(7) C(7) 116.71(10) yes . . . Cu(3) P(7) C(8) 117.75(11) yes . . . Cu(3) P(7) C(219) 115.45(11) yes . . . C(7) P(7) C(8) 97.04(15) yes . . . C(7) P(7) C(219) 102.20(15) yes . . . C(8) P(7) C(219) 105.01(14) yes . . . Cu(4) P(8) C(8) 118.19(11) yes . . . Cu(4) P(8) C(225) 113.08(11) yes . . . Cu(4) P(8) C(231) 113.60(11) yes . . . C(8) P(8) C(225) 104.84(14) yes . . . C(8) P(8) C(231) 102.38(15) yes . . . C(225) P(8) C(231) 103.09(15) yes . . . F(1) P(9) F(2) 90.59(19) yes . . . F(1) P(9) F(3) 87.68(18) yes . . . F(1) P(9) F(4) 175.2(2) yes . . . F(1) P(9) F(5) 88.95(18) yes . . . F(1) P(9) F(6) 93.8(2) yes . . . F(2) P(9) F(3) 88.68(18) yes . . . F(2) P(9) F(4) 90.4(2) yes . . . F(2) P(9) F(5) 179.17(19) yes . . . F(2) P(9) F(6) 90.0(2) yes . . . F(3) P(9) F(4) 87.69(19) yes . . . F(3) P(9) F(5) 90.62(16) yes . . . F(3) P(9) F(6) 178.0(2) yes . . . F(4) P(9) F(5) 90.0(2) yes . . . F(4) P(9) F(6) 90.8(2) yes . . . F(5) P(9) F(6) 90.7(2) yes . . . C(1) N(1) C(11) 178.4(3) yes . . . C(2) N(2) C(21) 177.4(4) yes . . . Cu(1) C(1) N(1) 174.7(3) yes . . . Cu(4) C(2) N(2) 177.3(3) yes . . . P(1) C(3) P(2) 116.01(17) yes . . . P(2) C(4) P(3) 114.88(16) yes . . . P(3) C(5) P(4) 114.38(17) yes . . . P(5) C(6) P(6) 116.26(18) yes . . . P(6) C(7) P(7) 115.61(17) yes . . . P(7) C(8) P(8) 115.04(18) yes . . . N(1) C(11) C(12) 117.8(3) yes . . . N(1) C(11) C(16) 118.5(3) yes . . . C(12) C(11) C(16) 123.7(3) yes . . . C(11) C(12) C(13) 116.6(4) yes . . . C(11) C(12) C(17) 121.8(3) yes . . . C(13) C(12) C(17) 121.6(3) yes . . . C(12) C(13) C(14) 121.2(4) yes . . . C(13) C(14) C(15) 120.9(4) yes . . . C(14) C(15) C(16) 120.9(4) yes . . . C(11) C(16) C(15) 116.6(3) yes . . . C(11) C(16) C(18) 121.4(3) yes . . . C(15) C(16) C(18) 122.0(3) yes . . . N(2) C(21) C(22) 118.3(5) yes . . . N(2) C(21) C(26) 115.4(5) yes . . . C(22) C(21) C(26) 126.3(6) yes . . . C(21) C(22) C(23) 115.9(6) yes . . . C(21) C(22) C(27) 121.9(6) yes . . . C(23) C(22) C(27) 122.1(6) yes . . . C(22) C(23) C(24) 114.5(7) yes . . . C(23) C(24) C(25) 127.1(10) yes . . . C(24) C(25) C(26) 121.4(9) yes . . . C(21) C(26) C(25) 114.7(7) yes . . . C(21) C(26) C(28) 123.4(6) yes . . . C(25) C(26) C(28) 121.9(7) yes . . . P(1) C(101) C(102) 119.6(2) yes . . . P(1) C(101) C(106) 121.7(2) yes . . . C(102) C(101) C(106) 118.7(3) yes . . . C(101) C(102) C(103) 120.6(3) yes . . . C(102) C(103) C(104) 120.2(4) yes . . . C(103) C(104) C(105) 119.4(4) yes . . . C(104) C(105) C(106) 120.7(4) yes . . . C(101) C(106) C(105) 120.3(3) yes . . . P(1) C(107) C(108) 121.7(2) yes . . . P(1) C(107) C(112) 119.1(2) yes . . . C(108) C(107) C(112) 119.1(3) yes . . . C(107) C(108) C(109) 120.1(3) yes . . . C(108) C(109) C(110) 120.7(4) yes . . . C(109) C(110) C(111) 119.9(4) yes . . . C(110) C(111) C(112) 120.0(4) yes . . . C(107) C(112) C(111) 120.2(3) yes . . . P(2) C(113) C(114) 121.5(2) yes . . . P(2) C(113) C(118) 119.6(2) yes . . . C(114) C(113) C(118) 118.9(3) yes . . . C(113) C(114) C(115) 120.8(3) yes . . . C(114) C(115) C(116) 119.9(3) yes . . . C(115) C(116) C(117) 120.0(3) yes . . . C(116) C(117) C(118) 120.1(3) yes . . . C(113) C(118) C(117) 120.3(3) yes . . . P(3) C(119) C(120) 123.0(2) yes . . . P(3) C(119) C(124) 118.4(2) yes . . . C(120) C(119) C(124) 118.6(3) yes . . . C(119) C(120) C(121) 120.8(3) yes . . . C(120) C(121) C(122) 119.6(4) yes . . . C(121) C(122) C(123) 119.6(4) yes . . . C(122) C(123) C(124) 121.3(4) yes . . . C(119) C(124) C(123) 120.0(3) yes . . . P(4) C(125) C(126) 123.1(3) yes . . . P(4) C(125) C(130) 117.8(2) yes . . . C(126) C(125) C(130) 118.9(3) yes . . . C(125) C(126) C(127) 120.4(4) yes . . . C(126) C(127) C(128) 120.2(4) yes . . . C(127) C(128) C(129) 120.2(4) yes . . . C(128) C(129) C(130) 120.0(4) yes . . . C(125) C(130) C(129) 120.4(3) yes . . . P(4) C(131) C(132) 117.2(2) yes . . . P(4) C(131) C(136) 124.4(2) yes . . . C(132) C(131) C(136) 118.4(3) yes . . . C(131) C(132) C(133) 120.8(3) yes . . . C(132) C(133) C(134) 120.4(3) yes . . . C(133) C(134) C(135) 119.3(3) yes . . . C(134) C(135) C(136) 120.8(3) yes . . . C(131) C(136) C(135) 120.3(3) yes . . . P(5) C(201) C(202) 123.9(3) yes . . . P(5) C(201) C(206) 118.0(2) yes . . . C(202) C(201) C(206) 118.1(3) yes . . . C(201) C(202) C(203) 120.3(4) yes . . . C(202) C(203) C(204) 120.5(5) yes . . . C(203) C(204) C(205) 119.6(5) yes . . . C(204) C(205) C(206) 120.2(4) yes . . . C(201) C(206) C(205) 121.3(3) yes . . . P(5) C(207) C(208) 117.7(2) yes . . . P(5) C(207) C(212) 123.3(2) yes . . . C(208) C(207) C(212) 119.0(3) yes . . . C(207) C(208) C(209) 120.3(3) yes . . . C(208) C(209) C(210) 120.4(3) yes . . . C(209) C(210) C(211) 119.5(3) yes . . . C(210) C(211) C(212) 120.6(4) yes . . . C(207) C(212) C(211) 120.1(3) yes . . . P(6) C(213) C(214) 118.3(2) yes . . . P(6) C(213) C(218) 122.4(2) yes . . . C(214) C(213) C(218) 119.2(3) yes . . . C(213) C(214) C(215) 119.6(3) yes . . . C(214) C(215) C(216) 120.6(3) yes . . . C(215) C(216) C(217) 120.2(3) yes . . . C(216) C(217) C(218) 120.0(4) yes . . . C(213) C(218) C(217) 120.4(3) yes . . . P(7) C(219) C(220) 118.4(2) yes . . . P(7) C(219) C(224) 122.0(2) yes . . . C(220) C(219) C(224) 119.4(3) yes . . . C(219) C(220) C(221) 120.2(3) yes . . . C(220) C(221) C(222) 120.1(3) yes . . . C(221) C(222) C(223) 120.2(4) yes . . . C(222) C(223) C(224) 120.4(4) yes . . . C(219) C(224) C(223) 119.8(3) yes . . . P(8) C(225) C(226) 118.7(2) yes . . . P(8) C(225) C(230) 122.3(2) yes . . . C(226) C(225) C(230) 118.9(3) yes . . . C(225) C(226) C(227) 119.9(3) yes . . . C(226) C(227) C(228) 120.6(4) yes . . . C(227) C(228) C(229) 119.8(4) yes . . . C(228) C(229) C(230) 120.3(4) yes . . . C(225) C(230) C(229) 120.5(3) yes . . . P(8) C(231) C(232) 120.2(2) yes . . . P(8) C(231) C(236) 121.2(2) yes . . . C(232) C(231) C(236) 118.3(3) yes . . . C(231) C(232) C(233) 120.7(3) yes . . . C(232) C(233) C(234) 120.3(3) yes . . . C(233) C(234) C(235) 119.6(3) yes . . . C(234) C(235) C(236) 119.9(3) yes . . . C(231) C(236) C(235) 121.1(3) yes . . . Cl(11) C(301) Cl(12) 113.5(5) yes . . . Cl(11) C(301) Cl(13) 104.9(5) yes . . . Cl(14) C(302) Cl(15) 123.6(15) yes . . . Cl(14) C(302) Cl(16) 101.9(7) yes . . . P(1) C(3) H(1) 107.8 no . . . P(1) C(3) H(2) 107.8 no . . . P(2) C(3) H(1) 108.2 no . . . P(2) C(3) H(2) 108.2 no . . . H(1) C(3) H(2) 108.6 no . . . P(2) C(4) H(3) 108.2 no . . . P(2) C(4) H(4) 108.4 no . . . P(3) C(4) H(3) 108.1 no . . . P(3) C(4) H(4) 108.2 no . . . H(3) C(4) H(4) 109.0 no . . . P(3) C(5) H(5) 108.6 no . . . P(3) C(5) H(6) 108.3 no . . . P(4) C(5) H(5) 108.6 no . . . P(4) C(5) H(6) 108.3 no . . . H(5) C(5) H(6) 108.5 no . . . P(5) C(6) H(7) 107.7 no . . . P(5) C(6) H(8) 107.7 no . . . P(6) C(6) H(7) 108.1 no . . . P(6) C(6) H(8) 108.1 no . . . H(7) C(6) H(8) 108.7 no . . . P(6) C(7) H(9) 108.0 no . . . P(6) C(7) H(10) 108.2 no . . . P(7) C(7) H(9) 107.9 no . . . P(7) C(7) H(10) 108.2 no . . . H(9) C(7) H(10) 108.7 no . . . P(7) C(8) H(11) 108.4 no . . . P(7) C(8) H(12) 108.2 no . . . P(8) C(8) H(11) 108.2 no . . . P(8) C(8) H(12) 107.9 no . . . H(11) C(8) H(12) 109.1 no . . . C(12) C(13) H(25) 119.2 no . . . C(14) C(13) H(25) 119.6 no . . . C(13) C(14) H(26) 118.9 no . . . C(15) C(14) H(26) 120.2 no . . . C(14) C(15) H(27) 119.2 no . . . C(16) C(15) H(27) 119.8 no . . . C(12) C(17) H(13) 110.3 no . . . C(12) C(17) H(14) 109.8 no . . . C(12) C(17) H(15) 110.0 no . . . H(13) C(17) H(14) 108.8 no . . . H(13) C(17) H(15) 109.3 no . . . H(14) C(17) H(15) 108.6 no . . . C(16) C(18) H(16) 110.5 no . . . C(16) C(18) H(17) 110.1 no . . . C(16) C(18) H(18) 110.7 no . . . H(16) C(18) H(17) 107.9 no . . . H(16) C(18) H(18) 109.2 no . . . H(17) C(18) H(18) 108.4 no . . . C(22) C(23) H(28) 112.8 no . . . C(24) C(23) H(28) 132.7 no . . . C(23) C(24) H(29) 103.9 no . . . C(25) C(24) H(29) 129.0 no . . . C(24) C(25) H(30) 114.9 no . . . C(26) C(25) H(30) 123.7 no . . . C(22) C(27) H(19) 113.9 no . . . C(22) C(27) H(20) 114.1 no . . . C(22) C(27) H(21) 116.2 no . . . H(19) C(27) H(20) 102.7 no . . . H(19) C(27) H(21) 104.4 no . . . H(20) C(27) H(21) 104.2 no . . . C(26) C(28) H(22) 115.0 no . . . C(26) C(28) H(23) 115.3 no . . . C(26) C(28) H(24) 112.9 no . . . H(22) C(28) H(23) 105.3 no . . . H(22) C(28) H(24) 103.2 no . . . H(23) C(28) H(24) 103.9 no . . . C(101) C(102) H(31) 119.4 no . . . C(103) C(102) H(31) 120.0 no . . . C(102) C(103) H(32) 119.8 no . . . C(104) C(103) H(32) 120.0 no . . . C(103) C(104) H(33) 119.8 no . . . C(105) C(104) H(33) 120.7 no . . . C(104) C(105) H(34) 118.9 no . . . C(106) C(105) H(34) 120.4 no . . . C(101) C(106) H(35) 119.8 no . . . C(105) C(106) H(35) 119.9 no . . . C(107) C(108) H(36) 119.8 no . . . C(109) C(108) H(36) 120.2 no . . . C(108) C(109) H(37) 119.7 no . . . C(110) C(109) H(37) 119.6 no . . . C(109) C(110) H(38) 119.7 no . . . C(111) C(110) H(38) 120.4 no . . . C(110) C(111) H(39) 119.7 no . . . C(112) C(111) H(39) 120.3 no . . . C(107) C(112) H(40) 119.6 no . . . C(111) C(112) H(40) 120.2 no . . . C(113) C(114) H(41) 119.2 no . . . C(115) C(114) H(41) 120.0 no . . . C(114) C(115) H(42) 119.8 no . . . C(116) C(115) H(42) 120.4 no . . . C(115) C(116) H(43) 119.9 no . . . C(117) C(116) H(43) 120.1 no . . . C(116) C(117) H(44) 119.8 no . . . C(118) C(117) H(44) 120.0 no . . . C(113) C(118) H(45) 119.5 no . . . C(117) C(118) H(45) 120.2 no . . . C(119) C(120) H(46) 119.1 no . . . C(121) C(120) H(46) 120.1 no . . . C(120) C(121) H(47) 119.6 no . . . C(122) C(121) H(47) 120.8 no . . . C(121) C(122) H(48) 120.4 no . . . C(123) C(122) H(48) 120.0 no . . . C(122) C(123) H(49) 119.4 no . . . C(124) C(123) H(49) 119.2 no . . . C(119) C(124) H(50) 119.5 no . . . C(123) C(124) H(50) 120.5 no . . . C(125) C(126) H(51) 119.1 no . . . C(127) C(126) H(51) 120.5 no . . . C(126) C(127) H(52) 119.7 no . . . C(128) C(127) H(52) 120.1 no . . . C(127) C(128) H(53) 119.9 no . . . C(129) C(128) H(53) 119.9 no . . . C(128) C(129) H(54) 120.3 no . . . C(130) C(129) H(54) 119.7 no . . . C(125) C(130) H(55) 119.1 no . . . C(129) C(130) H(55) 120.5 no . . . C(131) C(132) H(56) 119.5 no . . . C(133) C(132) H(56) 119.7 no . . . C(132) C(133) H(57) 119.7 no . . . C(134) C(133) H(57) 119.9 no . . . C(133) C(134) H(58) 120.6 no . . . C(135) C(134) H(58) 120.1 no . . . C(134) C(135) H(59) 120.0 no . . . C(136) C(135) H(59) 119.2 no . . . C(131) C(136) H(60) 119.9 no . . . C(135) C(136) H(60) 119.8 no . . . C(201) C(202) H(61) 119.6 no . . . C(203) C(202) H(61) 120.1 no . . . C(202) C(203) H(62) 119.5 no . . . C(204) C(203) H(62) 120.0 no . . . C(203) C(204) H(63) 119.4 no . . . C(205) C(204) H(63) 120.9 no . . . C(204) C(205) H(64) 119.9 no . . . C(206) C(205) H(64) 119.9 no . . . C(201) C(206) H(65) 119.3 no . . . C(205) C(206) H(65) 119.4 no . . . C(207) C(208) H(66) 119.9 no . . . C(209) C(208) H(66) 119.8 no . . . C(208) C(209) H(67) 119.8 no . . . C(210) C(209) H(67) 119.9 no . . . C(209) C(210) H(68) 120.8 no . . . C(211) C(210) H(68) 119.7 no . . . C(210) C(211) H(69) 119.7 no . . . C(212) C(211) H(69) 119.7 no . . . C(207) C(212) H(70) 119.6 no . . . C(211) C(212) H(70) 120.2 no . . . C(213) C(214) H(71) 119.8 no . . . C(215) C(214) H(71) 120.6 no . . . C(214) C(215) H(72) 119.9 no . . . C(216) C(215) H(72) 119.6 no . . . C(215) C(216) H(73) 120.0 no . . . C(217) C(216) H(73) 119.8 no . . . C(216) C(217) H(74) 120.0 no . . . C(218) C(217) H(74) 120.0 no . . . C(213) C(218) H(75) 119.5 no . . . C(217) C(218) H(75) 120.1 no . . . C(219) C(220) H(76) 120.0 no . . . C(221) C(220) H(76) 119.8 no . . . C(220) C(221) H(77) 120.0 no . . . C(222) C(221) H(77) 119.8 no . . . C(221) C(222) H(78) 119.7 no . . . C(223) C(222) H(78) 120.1 no . . . C(222) C(223) H(79) 120.2 no . . . C(224) C(223) H(79) 119.5 no . . . C(219) C(224) H(80) 119.6 no . . . C(223) C(224) H(80) 120.5 no . . . C(225) C(226) H(81) 119.8 no . . . C(227) C(226) H(81) 120.3 no . . . C(226) C(227) H(82) 119.4 no . . . C(228) C(227) H(82) 120.0 no . . . C(227) C(228) H(83) 120.1 no . . . C(229) C(228) H(83) 120.1 no . . . C(228) C(229) H(84) 119.6 no . . . C(230) C(229) H(84) 120.1 no . . . C(225) C(230) H(85) 119.5 no . . . C(229) C(230) H(85) 120.1 no . . . C(231) C(232) H(86) 119.6 no . . . C(233) C(232) H(86) 119.7 no . . . C(232) C(233) H(87) 119.6 no . . . C(234) C(233) H(87) 120.1 no . . . C(233) C(234) H(88) 120.1 no . . . C(235) C(234) H(88) 120.3 no . . . C(234) C(235) H(89) 120.2 no . . . C(236) C(235) H(89) 119.8 no . . . C(231) C(236) H(90) 119.8 no . . . C(235) C(236) H(90) 119.0 no . . . #============================================================================== #============================================================================== data__compound8b-revised #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731701' # CHEMICAL DATA _chemical_formula_sum 'C99 H96 Cl2 Cu4 F6 I3 N2 P9 ' _chemical_formula_moiety 'C99 H96 Cl2 Cu4 F6 I3 N2 P9 ' _chemical_formula_weight 2412.42 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z 3 -X,-Y,-Z 4 +X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 13.0832(4) _cell_length_b 30.7184(7) _cell_length_c 14.8956(4) _cell_angle_alpha 90.0000 _cell_angle_beta 105.2216(10) _cell_angle_gamma 90.0000 _cell_volume 5776.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11007 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2404.00 _exptl_absorpt_coefficient_mu 1.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.705 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 53143 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 13351 _reflns_number_gt 10726 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1400 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 13351 _refine_ls_number_parameters 587 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1261P)^2^+29.5004P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0110 _refine_diff_density_max 2.85 _refine_diff_density_min -0.98 _refine_ls_extinction_method none _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.13045(2) 0.113070(7) 0.427410(16) 0.03448(7) Uani 1.00 1 d . . . I(2) I 0.11454(3) 0.2500 0.47928(2) 0.02919(8) Uani 1.00 2 d S . . Cu(1) Cu 0.16770(3) 0.081370(13) 0.27233(3) 0.02733(10) Uani 1.00 1 d . . . Cu(2) Cu 0.14868(3) 0.192700(13) 0.35594(3) 0.02511(10) Uani 1.00 1 d . . . Cl(1) Cl 0.4040(5) 0.04089(16) 0.7279(3) 0.1315(19) Uani 0.50 1 d P . . Cl(2) Cl 0.2510(5) 0.1158(2) 0.7257(3) 0.158(2) Uani 0.50 1 d P . . P(1) P 0.33064(7) 0.10438(3) 0.26679(6) 0.02665(16) Uani 1.00 1 d . . . P(2) P 0.31596(6) 0.19849(3) 0.34576(6) 0.02331(15) Uani 1.00 1 d . . . P(3) P 0.03853(7) 0.10503(3) 0.14832(6) 0.02540(16) Uani 1.00 1 d . . . P(4) P 0.01550(6) 0.19847(2) 0.22707(6) 0.02181(15) Uani 1.00 1 d . . . P(5) P -0.1922(2) 0.2500 -0.12019(13) 0.0705(6) Uani 1.00 2 d S . . F(1) F -0.1188(6) 0.2866(2) -0.0717(4) 0.164(2) Uani 1.00 1 d . . . F(2) F -0.2456(8) 0.2500 -0.0348(4) 0.124(2) Uani 1.00 2 d S . . F(3) F -0.1482(8) 0.2500 -0.2060(4) 0.135(3) Uani 1.00 2 d S . . F(4) F -0.2723(5) 0.2866(2) -0.1659(4) 0.151(2) Uani 1.00 1 d . . . N(1) N 0.1553(2) -0.01787(10) 0.2992(2) 0.0326(6) Uani 1.00 1 d . . . C(1) C 0.1632(3) 0.01902(12) 0.2885(2) 0.0331(7) Uani 1.00 1 d . . . C(2) C 0.3531(2) 0.16299(11) 0.2592(2) 0.0284(6) Uani 1.00 1 d . . . C(3) C 0.3523(4) 0.2500 0.2976(3) 0.0270(8) Uani 1.00 2 d S . . C(4) C 0.0239(2) 0.16381(10) 0.1282(2) 0.0258(6) Uani 1.00 1 d . . . C(5) C 0.0105(4) 0.2500 0.1633(3) 0.0239(8) Uani 1.00 2 d S . . C(11) C 0.1400(2) -0.06116(11) 0.3188(2) 0.0307(6) Uani 1.00 1 d . . . C(12) C 0.1810(3) -0.09401(12) 0.2731(2) 0.0323(7) Uani 1.00 1 d . . . C(13) C 0.1618(3) -0.13670(11) 0.2946(2) 0.0346(7) Uani 1.00 1 d . . . C(14) C 0.1070(3) -0.14680(12) 0.3587(3) 0.0391(8) Uani 1.00 1 d . . . C(15) C 0.0681(4) -0.11317(13) 0.4037(3) 0.0503(11) Uani 1.00 1 d . . . C(16) C 0.0851(3) -0.07002(12) 0.3843(3) 0.0458(10) Uani 1.00 1 d . . . C(17) C 0.2393(4) -0.08302(16) 0.2025(3) 0.0567(12) Uani 1.00 1 d . . . C(18) C 0.0860(4) -0.19353(14) 0.3816(3) 0.0550(11) Uani 1.00 1 d . . . C(19) C 0.0430(6) -0.03359(17) 0.4315(5) 0.090(2) Uani 1.00 1 d . . . C(101) C 0.3623(2) 0.08311(12) 0.1632(2) 0.0336(7) Uani 1.00 1 d . . . C(102) C 0.3595(4) 0.10701(17) 0.0852(3) 0.0526(11) Uani 1.00 1 d . . . C(103) C 0.3724(4) 0.0873(2) 0.0034(3) 0.0621(13) Uani 1.00 1 d . . . C(104) C 0.3916(4) 0.0437(2) 0.0017(4) 0.0614(14) Uani 1.00 1 d . . . C(105) C 0.3961(4) 0.01880(18) 0.0809(4) 0.0591(13) Uani 1.00 1 d . . . C(106) C 0.3802(3) 0.03826(15) 0.1603(3) 0.0478(10) Uani 1.00 1 d . . . C(107) C 0.4441(3) 0.08583(12) 0.3583(2) 0.0379(8) Uani 1.00 1 d . . . C(108) C 0.4290(4) 0.0701(2) 0.4404(3) 0.0617(13) Uani 1.00 1 d . . . C(109) C 0.5169(6) 0.0570(3) 0.5116(4) 0.097(2) Uani 1.00 1 d . . . C(110) C 0.6158(5) 0.0588(2) 0.5014(4) 0.084(2) Uani 1.00 1 d . . . C(111) C 0.6319(4) 0.0745(2) 0.4198(5) 0.078(2) Uani 1.00 1 d . . . C(112) C 0.5460(3) 0.08776(16) 0.3468(3) 0.0543(11) Uani 1.00 1 d . . . C(113) C 0.4205(2) 0.19136(11) 0.4533(2) 0.0314(7) Uani 1.00 1 d . . . C(114) C 0.3893(3) 0.18777(19) 0.5360(3) 0.0513(11) Uani 1.00 1 d . . . C(115) C 0.4657(5) 0.1841(2) 0.6208(3) 0.0757(17) Uani 1.00 1 d . . . C(116) C 0.5714(4) 0.1831(2) 0.6220(3) 0.0705(16) Uani 1.00 1 d . . . C(117) C 0.6009(3) 0.1853(2) 0.5421(4) 0.0738(17) Uani 1.00 1 d . . . C(118) C 0.5256(3) 0.1905(2) 0.4575(3) 0.0556(12) Uani 1.00 1 d . . . C(119) C 0.0595(2) 0.08555(11) 0.0385(2) 0.0289(6) Uani 1.00 1 d . . . C(120) C 0.0970(3) 0.04351(13) 0.0358(2) 0.0378(8) Uani 1.00 1 d . . . C(121) C 0.1163(3) 0.02695(14) -0.0447(3) 0.0459(9) Uani 1.00 1 d . . . C(122) C 0.0994(3) 0.05209(15) -0.1233(3) 0.0441(9) Uani 1.00 1 d . . . C(123) C 0.0625(3) 0.09419(15) -0.1227(2) 0.0425(8) Uani 1.00 1 d . . . C(124) C 0.0415(3) 0.11088(12) -0.0432(2) 0.0371(8) Uani 1.00 1 d . . . C(125) C -0.0974(2) 0.08786(11) 0.1424(2) 0.0348(7) Uani 1.00 1 d . . . C(126) C -0.1172(3) 0.06794(15) 0.2181(3) 0.0500(10) Uani 1.00 1 d . . . C(127) C -0.2223(4) 0.0545(2) 0.2150(5) 0.0709(16) Uani 1.00 1 d . . . C(128) C -0.3020(3) 0.0623(2) 0.1369(5) 0.0736(18) Uani 1.00 1 d . . . C(129) C -0.2819(3) 0.08211(17) 0.0613(4) 0.0618(14) Uani 1.00 1 d . . . C(130) C -0.1796(3) 0.09480(14) 0.0616(3) 0.0464(9) Uani 1.00 1 d . . . C(131) C -0.1198(2) 0.19145(10) 0.2358(2) 0.0285(6) Uani 1.00 1 d . . . C(132) C -0.1354(3) 0.18384(17) 0.3230(3) 0.0468(10) Uani 1.00 1 d . . . C(133) C -0.2394(4) 0.1794(2) 0.3321(3) 0.0703(16) Uani 1.00 1 d . . . C(134) C -0.3240(3) 0.1830(2) 0.2551(4) 0.0642(14) Uani 1.00 1 d . . . C(135) C -0.3090(3) 0.18946(17) 0.1690(3) 0.0519(11) Uani 1.00 1 d . . . C(136) C -0.2064(3) 0.19353(14) 0.1585(3) 0.0399(8) Uani 1.00 1 d . . . C(201) C 0.3270(10) 0.0819(5) 0.6695(7) 0.077(3) Uani 0.50 1 d P . . H(1) H 0.1886 -0.1600 0.2646 0.041 Uiso 1.00 1 c R . . H(2) H 0.0306 -0.1200 0.4489 0.060 Uiso 1.00 1 c R . . H(3) H 0.2624 -0.1088 0.1783 0.069 Uiso 1.00 1 c R . . H(4) H 0.1964 -0.0665 0.1531 0.069 Uiso 1.00 1 c R . . H(5) H 0.3015 -0.0660 0.2313 0.069 Uiso 1.00 1 c R . . H(6) H 0.0120 -0.1985 0.3679 0.067 Uiso 1.00 1 c R . . H(7) H 0.1170 -0.2127 0.3466 0.067 Uiso 1.00 1 c R . . H(8) H 0.1167 -0.1987 0.4466 0.067 Uiso 1.00 1 c R . . H(9) H 0.0977 -0.0155 0.4639 0.107 Uiso 1.00 1 c R . . H(10) H -0.0072 -0.0167 0.3855 0.107 Uiso 1.00 1 c R . . H(11) H 0.0055 -0.0453 0.4736 0.107 Uiso 1.00 1 c R . . H(12) H 0.3485 0.1378 0.0862 0.064 Uiso 1.00 1 c R . . H(13) H 0.3690 0.1047 -0.0504 0.075 Uiso 1.00 1 c R . . H(14) H 0.4008 0.0299 -0.0541 0.073 Uiso 1.00 1 c R . . H(15) H 0.4113 -0.0117 0.0808 0.072 Uiso 1.00 1 c R . . H(16) H 0.3811 0.0210 0.2140 0.060 Uiso 1.00 1 c R . . H(17) H 0.3594 0.0675 0.4479 0.074 Uiso 1.00 1 c R . . H(18) H 0.5058 0.0463 0.5688 0.115 Uiso 1.00 1 c R . . H(19) H 0.6756 0.0518 0.5510 0.105 Uiso 1.00 1 c R . . H(20) H 0.7028 0.0760 0.4107 0.089 Uiso 1.00 1 c R . . H(21) H 0.5569 0.0984 0.2889 0.064 Uiso 1.00 1 c R . . H(22) H 0.3157 0.1893 0.5350 0.061 Uiso 1.00 1 c R . . H(23) H 0.4452 0.1796 0.6767 0.091 Uiso 1.00 1 c R . . H(24) H 0.6234 0.1822 0.6803 0.083 Uiso 1.00 1 c R . . H(25) H 0.6744 0.1830 0.5432 0.089 Uiso 1.00 1 c R . . H(26) H 0.5480 0.1927 0.4020 0.067 Uiso 1.00 1 c R . . H(27) H 0.1104 0.0258 0.0903 0.046 Uiso 1.00 1 c R . . H(28) H 0.1391 -0.0026 -0.0451 0.055 Uiso 1.00 1 c R . . H(29) H 0.1136 0.0404 -0.1785 0.053 Uiso 1.00 1 c R . . H(30) H 0.0524 0.1122 -0.1770 0.051 Uiso 1.00 1 c R . . H(31) H 0.0124 0.1395 -0.0437 0.045 Uiso 1.00 1 c R . . H(32) H -0.0613 0.0635 0.2740 0.062 Uiso 1.00 1 c R . . H(33) H -0.2375 0.0401 0.2666 0.084 Uiso 1.00 1 c R . . H(34) H -0.3719 0.0527 0.1366 0.085 Uiso 1.00 1 c R . . H(35) H -0.3393 0.0870 0.0081 0.076 Uiso 1.00 1 c R . . H(36) H -0.1661 0.1078 0.0073 0.057 Uiso 1.00 1 c R . . H(37) H -0.0758 0.1814 0.3760 0.056 Uiso 1.00 1 c R . . H(38) H -0.2499 0.1741 0.3927 0.083 Uiso 1.00 1 c R . . H(39) H -0.3942 0.1798 0.2613 0.075 Uiso 1.00 1 c R . . H(40) H -0.3681 0.1909 0.1150 0.062 Uiso 1.00 1 c R . . H(41) H -0.1959 0.1981 0.0981 0.048 Uiso 1.00 1 c R . . H(42) H 0.4270 0.1671 0.2651 0.035 Uiso 1.00 1 c R . . H(43) H 0.3144 0.1724 0.1989 0.035 Uiso 1.00 1 c R . . H(44) H 0.0836 0.1734 0.1078 0.032 Uiso 1.00 1 c R . . H(45) H -0.0387 0.1683 0.0795 0.032 Uiso 1.00 1 c R . . H(46) H 0.4251 0.2500 0.2984 0.033 Uiso 1.00 2 c R . . H(47) H 0.3108 0.2500 0.2345 0.033 Uiso 1.00 2 c R . . H(48) H 0.0726 0.2500 0.1420 0.029 Uiso 1.00 2 c R . . H(49) H -0.0500 0.2500 0.1106 0.029 Uiso 1.00 2 c R . . H(50) H 0.3772 0.1007 0.6502 0.092 Uiso 0.50 1 c R . . H(51) H 0.2816 0.0696 0.6155 0.092 Uiso 0.50 1 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.05037(16) 0.02464(13) 0.03443(13) 0.00101(9) 0.02176(11) 0.00423(8) I(2) 0.03697(18) 0.02551(15) 0.02853(16) 0.0000 0.01468(12) 0.0000 Cu(1) 0.0311(2) 0.01895(19) 0.0333(2) -0.00006(15) 0.01071(17) 0.00151(15) Cu(2) 0.0251(2) 0.0248(2) 0.0263(2) 0.00026(14) 0.00848(15) 0.00163(14) Cl(1) 0.216(5) 0.096(3) 0.091(2) 0.006(3) 0.055(3) 0.047(2) Cl(2) 0.136(4) 0.274(9) 0.082(2) 0.024(4) 0.061(3) 0.009(3) P(1) 0.0269(4) 0.0207(3) 0.0331(4) 0.0018(3) 0.0091(3) -0.0023(3) P(2) 0.0236(3) 0.0194(3) 0.0272(3) 0.0014(2) 0.0072(3) -0.0001(2) P(3) 0.0267(4) 0.0185(3) 0.0312(4) -0.0007(2) 0.0081(3) -0.0024(3) P(4) 0.0234(3) 0.0172(3) 0.0258(3) -0.0003(2) 0.0083(2) 0.0002(2) P(5) 0.1210(19) 0.0506(10) 0.0325(8) 0.0000 0.0070(9) 0.0000 F(1) 0.229(7) 0.120(4) 0.140(4) -0.074(4) 0.041(4) -0.061(3) F(2) 0.243(9) 0.081(3) 0.063(3) 0.0000 0.068(4) 0.0000 F(3) 0.234(9) 0.124(5) 0.065(3) 0.0000 0.072(4) 0.0000 F(4) 0.176(5) 0.166(5) 0.120(4) 0.091(4) 0.054(3) 0.075(3) N(1) 0.0387(16) 0.0224(14) 0.0372(15) -0.0008(11) 0.0107(12) 0.0025(11) C(1) 0.0383(18) 0.0256(16) 0.0377(17) 0.0010(13) 0.0143(14) 0.0010(13) C(2) 0.0301(16) 0.0244(15) 0.0335(16) -0.0011(12) 0.0136(13) -0.0037(12) C(3) 0.028(2) 0.020(2) 0.035(2) 0.0000 0.0121(18) 0.0000 C(4) 0.0293(15) 0.0205(14) 0.0278(14) -0.0006(11) 0.0078(12) -0.0019(11) C(5) 0.029(2) 0.0185(19) 0.026(2) 0.0000 0.0107(16) 0.0000 C(11) 0.0355(17) 0.0199(15) 0.0371(17) -0.0007(12) 0.0105(14) -0.0004(12) C(12) 0.0387(18) 0.0252(16) 0.0348(17) 0.0004(13) 0.0127(14) 0.0002(13) C(13) 0.0380(18) 0.0221(16) 0.0440(19) 0.0002(13) 0.0115(15) -0.0036(13) C(14) 0.048(2) 0.0219(16) 0.049(2) -0.0020(14) 0.0139(17) 0.0029(14) C(15) 0.078(3) 0.0270(19) 0.060(2) -0.0065(18) 0.043(2) -0.0015(17) C(16) 0.067(2) 0.0222(17) 0.062(2) -0.0041(17) 0.042(2) -0.0062(16) C(17) 0.083(3) 0.043(2) 0.060(2) -0.006(2) 0.047(2) -0.005(2) C(18) 0.074(3) 0.0236(18) 0.070(3) -0.0087(19) 0.025(2) 0.0058(18) C(19) 0.149(6) 0.037(2) 0.126(5) -0.000(3) 0.112(5) -0.013(3) C(101) 0.0273(16) 0.0308(17) 0.0444(19) -0.0020(13) 0.0124(14) -0.0131(14) C(102) 0.069(3) 0.048(2) 0.046(2) -0.001(2) 0.026(2) -0.0095(19) C(103) 0.068(3) 0.072(3) 0.056(2) 0.003(2) 0.034(2) -0.014(2) C(104) 0.050(2) 0.070(3) 0.069(3) -0.007(2) 0.025(2) -0.039(2) C(105) 0.051(2) 0.054(2) 0.077(3) 0.000(2) 0.025(2) -0.037(2) C(106) 0.041(2) 0.040(2) 0.063(2) 0.0039(17) 0.0153(19) -0.0151(19) C(107) 0.0371(19) 0.0268(17) 0.045(2) 0.0078(14) 0.0020(15) -0.0044(14) C(108) 0.061(3) 0.072(3) 0.048(2) 0.027(2) 0.007(2) 0.014(2) C(109) 0.102(5) 0.123(6) 0.051(3) 0.046(4) -0.005(3) 0.019(3) C(110) 0.065(3) 0.103(5) 0.067(3) 0.038(3) -0.014(2) -0.005(3) C(111) 0.040(2) 0.071(3) 0.107(5) 0.013(2) -0.009(2) -0.026(3) C(112) 0.036(2) 0.047(2) 0.074(3) 0.0037(18) 0.002(2) -0.009(2) C(113) 0.0315(17) 0.0248(15) 0.0350(17) 0.0050(12) 0.0035(13) -0.0004(12) C(114) 0.040(2) 0.076(3) 0.035(2) 0.013(2) 0.0053(17) 0.008(2) C(115) 0.065(3) 0.117(5) 0.038(2) 0.015(3) 0.000(2) 0.008(2) C(116) 0.063(3) 0.090(4) 0.043(2) 0.014(2) -0.014(2) 0.007(2) C(117) 0.031(2) 0.117(5) 0.063(3) 0.011(2) -0.007(2) 0.004(3) C(118) 0.037(2) 0.086(3) 0.043(2) 0.003(2) 0.0075(17) 0.002(2) C(119) 0.0270(15) 0.0250(15) 0.0351(16) -0.0014(12) 0.0093(12) -0.0067(12) C(120) 0.042(2) 0.0289(17) 0.0427(19) 0.0028(15) 0.0116(16) -0.0060(15) C(121) 0.052(2) 0.037(2) 0.050(2) 0.0057(17) 0.0160(19) -0.0156(18) C(122) 0.040(2) 0.049(2) 0.045(2) 0.0016(17) 0.0135(16) -0.0184(18) C(123) 0.046(2) 0.049(2) 0.0320(18) 0.0050(18) 0.0102(16) -0.0062(16) C(124) 0.048(2) 0.0326(18) 0.0297(17) 0.0069(15) 0.0083(15) -0.0022(13) C(125) 0.0333(17) 0.0225(15) 0.051(2) -0.0030(13) 0.0157(15) -0.0119(14) C(126) 0.048(2) 0.043(2) 0.068(2) -0.0152(19) 0.031(2) -0.011(2) C(127) 0.062(3) 0.065(3) 0.101(4) -0.027(2) 0.049(3) -0.022(3) C(128) 0.033(2) 0.066(3) 0.127(5) -0.022(2) 0.032(2) -0.043(3) C(129) 0.036(2) 0.051(2) 0.094(4) -0.010(2) 0.009(2) -0.027(2) C(130) 0.039(2) 0.033(2) 0.063(2) -0.0029(16) 0.0060(18) -0.0111(18) C(131) 0.0291(16) 0.0203(14) 0.0387(17) -0.0014(11) 0.0135(13) -0.0008(12) C(132) 0.039(2) 0.066(2) 0.040(2) -0.0143(19) 0.0197(17) -0.0085(19) C(133) 0.052(2) 0.111(5) 0.059(2) -0.022(3) 0.034(2) -0.013(3) C(134) 0.028(2) 0.086(3) 0.086(3) -0.014(2) 0.028(2) -0.016(3) C(135) 0.0233(18) 0.057(2) 0.073(3) -0.0048(17) 0.0077(18) 0.003(2) C(136) 0.0307(18) 0.041(2) 0.048(2) -0.0026(15) 0.0089(15) 0.0068(16) C(201) 0.072(7) 0.118(11) 0.043(5) 0.007(7) 0.019(5) -0.010(6) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Cu(1) 2.6670(5) yes . . I(1) Cu(2) 2.7031(4) yes . . I(2) Cu(2) 2.6653(5) yes . . I(2) Cu(2) 2.6653(5) yes . 4_555 Cu(1) P(1) 2.2679(10) yes . . Cu(1) P(3) 2.2709(8) yes . . Cu(1) C(1) 1.933(3) yes . . Cu(2) P(2) 2.2402(9) yes . . Cu(2) P(4) 2.2352(8) yes . . Cl(1) C(201) 1.702(15) yes . . Cl(2) C(201) 1.793(16) yes . . P(1) C(2) 1.833(3) yes . . P(1) C(101) 1.821(4) yes . . P(1) C(107) 1.823(3) yes . . P(2) C(2) 1.849(3) yes . . P(2) C(3) 1.850(2) yes . . P(2) C(113) 1.826(3) yes . . P(3) C(4) 1.832(3) yes . . P(3) C(119) 1.829(4) yes . . P(3) C(125) 1.835(3) yes . . P(4) C(4) 1.844(3) yes . . P(4) C(5) 1.838(2) yes . . P(4) C(131) 1.822(3) yes . . P(5) F(1) 1.530(6) yes . . P(5) F(1) 1.530(6) yes . 4_555 P(5) F(2) 1.604(8) yes . . P(5) F(3) 1.533(8) yes . . P(5) F(4) 1.565(6) yes . . P(5) F(4) 1.565(6) yes . 4_555 N(1) C(1) 1.153(4) yes . . N(1) C(11) 1.387(4) yes . . C(11) C(12) 1.401(5) yes . . C(11) C(16) 1.382(7) yes . . C(12) C(13) 1.388(5) yes . . C(12) C(17) 1.490(7) yes . . C(13) C(14) 1.372(6) yes . . C(14) C(15) 1.398(6) yes . . C(14) C(18) 1.517(5) yes . . C(15) C(16) 1.387(5) yes . . C(16) C(19) 1.501(8) yes . . C(101) C(102) 1.366(6) yes . . C(101) C(106) 1.400(5) yes . . C(102) C(103) 1.410(8) yes . . C(103) C(104) 1.365(8) yes . . C(104) C(105) 1.394(8) yes . . C(105) C(106) 1.390(8) yes . . C(107) C(108) 1.377(7) yes . . C(107) C(112) 1.389(6) yes . . C(108) C(109) 1.402(8) yes . . C(109) C(110) 1.344(11) yes . . C(110) C(111) 1.373(11) yes . . C(111) C(112) 1.405(7) yes . . C(113) C(114) 1.399(6) yes . . C(113) C(118) 1.361(6) yes . . C(114) C(115) 1.395(6) yes . . C(115) C(116) 1.379(9) yes . . C(116) C(117) 1.346(8) yes . . C(117) C(118) 1.390(6) yes . . C(119) C(120) 1.386(5) yes . . C(119) C(124) 1.411(5) yes . . C(120) C(121) 1.385(6) yes . . C(121) C(122) 1.372(6) yes . . C(122) C(123) 1.381(6) yes . . C(123) C(124) 1.382(6) yes . . C(125) C(126) 1.366(7) yes . . C(125) C(130) 1.404(5) yes . . C(126) C(127) 1.424(8) yes . . C(127) C(128) 1.364(8) yes . . C(128) C(129) 1.365(10) yes . . C(129) C(130) 1.392(6) yes . . C(131) C(132) 1.386(6) yes . . C(131) C(136) 1.390(4) yes . . C(132) C(133) 1.409(7) yes . . C(133) C(134) 1.372(6) yes . . C(134) C(135) 1.363(8) yes . . C(135) C(136) 1.397(6) yes . . C(2) H(42) 0.956 no . . C(2) H(43) 0.953 no . . C(3) H(46) 0.949 no . . C(3) H(47) 0.954 no . . C(4) H(44) 0.955 no . . C(4) H(45) 0.951 no . . C(5) H(48) 0.947 no . . C(5) H(49) 0.958 no . . C(13) H(1) 0.957 no . . C(15) H(2) 0.954 no . . C(17) H(3) 0.953 no . . C(17) H(4) 0.948 no . . C(17) H(5) 0.968 no . . C(18) H(6) 0.947 no . . C(18) H(7) 0.947 no . . C(18) H(8) 0.958 no . . C(19) H(9) 0.934 no . . C(19) H(10) 0.967 no . . C(19) H(11) 0.962 no . . C(102) H(12) 0.956 no . . C(103) H(13) 0.955 no . . C(104) H(14) 0.967 no . . C(105) H(15) 0.957 no . . C(106) H(16) 0.958 no . . C(108) H(17) 0.950 no . . C(109) H(18) 0.958 no . . C(110) H(19) 0.949 no . . C(111) H(20) 0.974 no . . C(112) H(21) 0.967 no . . C(114) H(22) 0.960 no . . C(115) H(23) 0.950 no . . C(116) H(24) 0.952 no . . C(117) H(25) 0.961 no . . C(118) H(26) 0.949 no . . C(120) H(27) 0.955 no . . C(121) H(28) 0.954 no . . C(122) H(29) 0.959 no . . C(123) H(30) 0.960 no . . C(124) H(31) 0.956 no . . C(126) H(32) 0.963 no . . C(127) H(33) 0.953 no . . C(128) H(34) 0.960 no . . C(129) H(35) 0.949 no . . C(130) H(36) 0.959 no . . C(132) H(37) 0.957 no . . C(133) H(38) 0.962 no . . C(134) H(39) 0.952 no . . C(135) H(40) 0.959 no . . C(136) H(41) 0.956 no . . C(201) H(50) 0.972 no . . C(201) H(51) 0.946 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) I(1) Cu(2) 86.227(15) yes . . . Cu(2) I(2) Cu(2) 82.660(16) yes . . 4_555 I(1) Cu(1) P(1) 107.76(2) yes . . . I(1) Cu(1) P(3) 108.75(2) yes . . . I(1) Cu(1) C(1) 103.63(12) yes . . . P(1) Cu(1) P(3) 112.12(3) yes . . . P(1) Cu(1) C(1) 111.89(12) yes . . . P(3) Cu(1) C(1) 112.20(10) yes . . . I(1) Cu(2) I(2) 106.143(17) yes . . . I(1) Cu(2) P(2) 106.70(2) yes . . . I(1) Cu(2) P(4) 106.29(2) yes . . . I(2) Cu(2) P(2) 109.74(2) yes . . . I(2) Cu(2) P(4) 107.80(2) yes . . . P(2) Cu(2) P(4) 119.39(3) yes . . . Cu(1) P(1) C(2) 118.42(12) yes . . . Cu(1) P(1) C(101) 110.13(11) yes . . . Cu(1) P(1) C(107) 117.64(14) yes . . . C(2) P(1) C(101) 102.95(17) yes . . . C(2) P(1) C(107) 103.96(15) yes . . . C(101) P(1) C(107) 101.53(18) yes . . . Cu(2) P(2) C(2) 116.15(11) yes . . . Cu(2) P(2) C(3) 116.69(15) yes . . . Cu(2) P(2) C(113) 116.81(13) yes . . . C(2) P(2) C(3) 95.31(18) yes . . . C(2) P(2) C(113) 105.54(16) yes . . . C(3) P(2) C(113) 103.49(17) yes . . . Cu(1) P(3) C(4) 118.16(9) yes . . . Cu(1) P(3) C(119) 111.64(11) yes . . . Cu(1) P(3) C(125) 116.87(12) yes . . . C(4) P(3) C(119) 102.09(15) yes . . . C(4) P(3) C(125) 102.56(15) yes . . . C(119) P(3) C(125) 103.53(17) yes . . . Cu(2) P(4) C(4) 116.33(10) yes . . . Cu(2) P(4) C(5) 115.21(13) yes . . . Cu(2) P(4) C(131) 118.82(11) yes . . . C(4) P(4) C(5) 94.92(16) yes . . . C(4) P(4) C(131) 104.60(15) yes . . . C(5) P(4) C(131) 103.63(19) yes . . . F(1) P(5) F(1) 94.4(3) yes . . 4_555 F(1) P(5) F(2) 88.6(3) yes . . . F(1) P(5) F(3) 93.9(3) yes . . . F(1) P(5) F(4) 86.8(3) yes . . . F(1) P(5) F(4) 176.3(4) yes . . 4_555 F(1) P(5) F(2) 88.6(3) yes 4_555 . . F(1) P(5) F(3) 93.9(3) yes 4_555 . . F(1) P(5) F(4) 176.3(4) yes 4_555 . . F(1) P(5) F(4) 86.8(3) yes 4_555 . 4_555 F(2) P(5) F(3) 176.4(4) yes . . . F(2) P(5) F(4) 87.9(3) yes . . . F(2) P(5) F(4) 87.9(3) yes . . 4_555 F(3) P(5) F(4) 89.5(3) yes . . . F(3) P(5) F(4) 89.5(3) yes . . 4_555 F(4) P(5) F(4) 91.8(3) yes . . 4_555 C(1) N(1) C(11) 174.0(4) yes . . . Cu(1) C(1) N(1) 176.3(3) yes . . . P(1) C(2) P(2) 117.4(2) yes . . . P(2) C(3) P(2) 117.6(2) yes . . 4_555 P(3) C(4) P(4) 117.62(18) yes . . . P(4) C(5) P(4) 118.9(2) yes . . 4_555 N(1) C(11) C(12) 119.5(3) yes . . . N(1) C(11) C(16) 117.9(3) yes . . . C(12) C(11) C(16) 122.5(3) yes . . . C(11) C(12) C(13) 116.9(3) yes . . . C(11) C(12) C(17) 120.8(3) yes . . . C(13) C(12) C(17) 122.2(3) yes . . . C(12) C(13) C(14) 122.2(3) yes . . . C(13) C(14) C(15) 119.3(3) yes . . . C(13) C(14) C(18) 122.0(4) yes . . . C(15) C(14) C(18) 118.7(4) yes . . . C(14) C(15) C(16) 120.5(5) yes . . . C(11) C(16) C(15) 118.5(4) yes . . . C(11) C(16) C(19) 120.4(4) yes . . . C(15) C(16) C(19) 121.1(5) yes . . . P(1) C(101) C(102) 124.5(3) yes . . . P(1) C(101) C(106) 117.1(3) yes . . . C(102) C(101) C(106) 118.1(4) yes . . . C(101) C(102) C(103) 121.4(4) yes . . . C(102) C(103) C(104) 120.2(5) yes . . . C(103) C(104) C(105) 119.3(5) yes . . . C(104) C(105) C(106) 120.2(5) yes . . . C(101) C(106) C(105) 120.8(4) yes . . . P(1) C(107) C(108) 119.8(3) yes . . . P(1) C(107) C(112) 120.9(3) yes . . . C(108) C(107) C(112) 119.3(4) yes . . . C(107) C(108) C(109) 119.5(5) yes . . . C(108) C(109) C(110) 121.7(6) yes . . . C(109) C(110) C(111) 119.4(5) yes . . . C(110) C(111) C(112) 120.6(5) yes . . . C(107) C(112) C(111) 119.4(5) yes . . . P(2) C(113) C(114) 117.2(2) yes . . . P(2) C(113) C(118) 123.9(3) yes . . . C(114) C(113) C(118) 118.9(3) yes . . . C(113) C(114) C(115) 119.9(4) yes . . . C(114) C(115) C(116) 119.4(5) yes . . . C(115) C(116) C(117) 120.5(4) yes . . . C(116) C(117) C(118) 120.6(5) yes . . . C(113) C(118) C(117) 120.7(4) yes . . . P(3) C(119) C(120) 117.9(2) yes . . . P(3) C(119) C(124) 124.1(2) yes . . . C(120) C(119) C(124) 118.0(3) yes . . . C(119) C(120) C(121) 120.9(3) yes . . . C(120) C(121) C(122) 120.5(4) yes . . . C(121) C(122) C(123) 120.0(4) yes . . . C(122) C(123) C(124) 120.1(3) yes . . . C(119) C(124) C(123) 120.5(3) yes . . . P(3) C(125) C(126) 118.7(2) yes . . . P(3) C(125) C(130) 120.8(3) yes . . . C(126) C(125) C(130) 120.5(3) yes . . . C(125) C(126) C(127) 119.5(4) yes . . . C(126) C(127) C(128) 119.6(6) yes . . . C(127) C(128) C(129) 120.8(5) yes . . . C(128) C(129) C(130) 121.0(4) yes . . . C(125) C(130) C(129) 118.6(4) yes . . . P(4) C(131) C(132) 118.2(2) yes . . . P(4) C(131) C(136) 122.1(3) yes . . . C(132) C(131) C(136) 119.7(3) yes . . . C(131) C(132) C(133) 119.3(3) yes . . . C(132) C(133) C(134) 119.9(5) yes . . . C(133) C(134) C(135) 121.0(4) yes . . . C(134) C(135) C(136) 119.8(3) yes . . . C(131) C(136) C(135) 120.1(4) yes . . . Cl(1) C(201) Cl(2) 121.2(7) yes . . . P(1) C(2) H(42) 107.5 no . . . P(1) C(2) H(43) 107.7 no . . . P(2) C(2) H(42) 107.6 no . . . P(2) C(2) H(43) 107.8 no . . . H(42) C(2) H(43) 108.7 no . . . P(2) C(3) H(46) 110.7 no . . . P(2) C(3) H(47) 104.2 no . . . P(2) C(3) H(46) 110.7 no 4_555 . . P(2) C(3) H(47) 104.2 no 4_555 . . H(46) C(3) H(47) 108.8 no . . . P(3) C(4) H(44) 107.3 no . . . P(3) C(4) H(45) 107.5 no . . . P(4) C(4) H(44) 107.5 no . . . P(4) C(4) H(45) 107.7 no . . . H(44) C(4) H(45) 108.9 no . . . P(4) C(5) H(48) 104.8 no . . . P(4) C(5) H(49) 109.5 no . . . P(4) C(5) H(48) 104.8 no 4_555 . . P(4) C(5) H(49) 109.5 no 4_555 . . H(48) C(5) H(49) 108.8 no . . . C(12) C(13) H(1) 119.2 no . . . C(14) C(13) H(1) 118.5 no . . . C(14) C(15) H(2) 119.7 no . . . C(16) C(15) H(2) 119.8 no . . . C(12) C(17) H(3) 110.6 no . . . C(12) C(17) H(4) 111.2 no . . . C(12) C(17) H(5) 109.7 no . . . H(3) C(17) H(4) 109.5 no . . . H(3) C(17) H(5) 107.7 no . . . H(4) C(17) H(5) 108.1 no . . . C(14) C(18) H(6) 109.8 no . . . C(14) C(18) H(7) 109.6 no . . . C(14) C(18) H(8) 109.4 no . . . H(6) C(18) H(7) 110.0 no . . . H(6) C(18) H(8) 109.0 no . . . H(7) C(18) H(8) 109.0 no . . . C(16) C(19) H(9) 111.2 no . . . C(16) C(19) H(10) 109.4 no . . . C(16) C(19) H(11) 109.8 no . . . H(9) C(19) H(10) 109.4 no . . . H(9) C(19) H(11) 109.9 no . . . H(10) C(19) H(11) 107.1 no . . . C(101) C(102) H(12) 119.3 no . . . C(103) C(102) H(12) 119.3 no . . . C(102) C(103) H(13) 119.7 no . . . C(104) C(103) H(13) 120.1 no . . . C(103) C(104) H(14) 120.6 no . . . C(105) C(104) H(14) 120.1 no . . . C(104) C(105) H(15) 119.9 no . . . C(106) C(105) H(15) 119.9 no . . . C(101) C(106) H(16) 119.0 no . . . C(105) C(106) H(16) 120.1 no . . . C(107) C(108) H(17) 119.8 no . . . C(109) C(108) H(17) 120.6 no . . . C(108) C(109) H(18) 119.0 no . . . C(110) C(109) H(18) 119.3 no . . . C(109) C(110) H(19) 121.6 no . . . C(111) C(110) H(19) 118.8 no . . . C(110) C(111) H(20) 121.0 no . . . C(112) C(111) H(20) 118.4 no . . . C(107) C(112) H(21) 119.7 no . . . C(111) C(112) H(21) 120.9 no . . . C(113) C(114) H(22) 120.4 no . . . C(115) C(114) H(22) 119.6 no . . . C(114) C(115) H(23) 120.4 no . . . C(116) C(115) H(23) 120.0 no . . . C(115) C(116) H(24) 119.1 no . . . C(117) C(116) H(24) 120.4 no . . . C(116) C(117) H(25) 119.9 no . . . C(118) C(117) H(25) 119.5 no . . . C(113) C(118) H(26) 119.9 no . . . C(117) C(118) H(26) 119.4 no . . . C(119) C(120) H(27) 119.6 no . . . C(121) C(120) H(27) 119.5 no . . . C(120) C(121) H(28) 118.9 no . . . C(122) C(121) H(28) 120.6 no . . . C(121) C(122) H(29) 119.8 no . . . C(123) C(122) H(29) 120.2 no . . . C(122) C(123) H(30) 120.3 no . . . C(124) C(123) H(30) 119.6 no . . . C(119) C(124) H(31) 119.3 no . . . C(123) C(124) H(31) 120.1 no . . . C(125) C(126) H(32) 120.8 no . . . C(127) C(126) H(32) 119.7 no . . . C(126) C(127) H(33) 120.8 no . . . C(128) C(127) H(33) 119.6 no . . . C(127) C(128) H(34) 117.6 no . . . C(129) C(128) H(34) 121.6 no . . . C(128) C(129) H(35) 118.5 no . . . C(130) C(129) H(35) 120.4 no . . . C(125) C(130) H(36) 121.1 no . . . C(129) C(130) H(36) 120.3 no . . . C(131) C(132) H(37) 119.9 no . . . C(133) C(132) H(37) 120.8 no . . . C(132) C(133) H(38) 119.1 no . . . C(134) C(133) H(38) 121.0 no . . . C(133) C(134) H(39) 119.9 no . . . C(135) C(134) H(39) 119.1 no . . . C(134) C(135) H(40) 120.9 no . . . C(136) C(135) H(40) 119.3 no . . . C(131) C(136) H(41) 119.9 no . . . C(135) C(136) H(41) 120.0 no . . . Cl(1) C(201) H(50) 103.6 no . . . Cl(1) C(201) H(51) 107.0 no . . . Cl(2) C(201) H(50) 107.2 no . . . Cl(2) C(201) H(51) 109.2 no . . . H(50) C(201) H(51) 108.0 no . . . # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.353 0.250 0.897 379 32 ' ' 2 0.275 0.750 0.540 10 0 ' ' 3 0.647 0.750 0.103 379 32 ' ' 4 0.724 0.250 0.459 10 0 ' ' _platon_squeeze_details ; ; #============================================================================== #============================================================================== data__compound9-revised2 #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 731702' # CHEMICAL DATA _chemical_formula_sum 'C89 H92 Cl2 Cu8 F12 I6 N2 O2 P10 ' _chemical_formula_moiety 'C89 H92 Cl2 Cu8 F12 I6 N2 O2 P10 ' _chemical_formula_weight 3100.14 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 11.619(4) _cell_length_b 15.852(5) _cell_length_c 16.931(6) _cell_angle_alpha 66.862(10) _cell_angle_beta 83.535(14) _cell_angle_gamma 71.204(10) _cell_volume 2714.2(15) _cell_formula_units_Z 1 _cell_measurement_reflns_used 6212 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153(2) #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1498.00 _exptl_absorpt_coefficient_mu 3.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_T_max 0.591 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 24968 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11882 _reflns_number_gt 10050 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1771 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 11882 _refine_ls_number_parameters 578 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0928P)^2^+20.2289P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0100 _refine_diff_density_max 1.71 _refine_diff_density_min -1.55 _refine_ls_extinction_method none _refine_ls_extinction_coef none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.87653(4) 0.36950(3) 0.50211(4) 0.04705(14) Uani 1.00 1 d . . . I(2) I 1.18024(4) 0.11802(3) 0.53276(3) 0.03412(13) Uani 1.00 1 d . . . I(3) I 0.82627(4) 0.12076(3) 0.50185(3) 0.03195(12) Uani 1.00 1 d . . . Cu(1) Cu 1.11354(10) 0.32666(8) 0.48067(8) 0.0574(2) Uani 1.00 1 d . . . Cu(2) Cu 0.96508(8) 0.18654(7) 0.59968(5) 0.0407(2) Uani 1.00 1 d . . . Cu(3) Cu 0.96577(8) 0.23321(6) 0.43322(5) 0.03654(18) Uani 1.00 1 d . . . Cu(4) Cu 1.04617(8) -0.00578(6) 0.57785(5) 0.03695(18) Uani 1.00 1 d . . . Cl(1) Cl 0.5039(5) 0.1216(5) 0.3786(6) 0.101(2) Uani 0.50 1 d P . . Cl(2) Cl 0.4113(6) -0.0191(5) 0.3727(5) 0.0979(19) Uani 0.50 1 d P . . P(1) P 1.16739(17) 0.37878(15) 0.34208(19) 0.0556(5) Uani 1.00 1 d . . . P(2) P 1.03416(15) 0.26146(12) 0.30057(11) 0.0329(3) Uani 1.00 1 d . . . P(3) P 0.99744(15) -0.07796(12) 0.71460(10) 0.0320(3) Uani 1.00 1 d . . . P(4) P 0.92310(15) 0.11813(13) 0.73776(10) 0.0339(3) Uani 1.00 1 d . . . P(11) P 1.33695(19) 0.1813(2) 0.06411(15) 0.0562(5) Uani 1.00 1 d . . . F(1) F 1.2392(12) 0.1281(10) 0.0812(9) 0.168(4) Uiso 1.00 1 d . . . F(2) F 1.4008(14) 0.2694(10) 0.0159(10) 0.179(5) Uiso 1.00 1 d . . . F(3) F 1.2198(14) 0.2642(11) 0.0643(10) 0.186(5) Uiso 1.00 1 d . . . F(4) F 1.3252(11) 0.2106(8) -0.0307(8) 0.145(3) Uiso 1.00 1 d . . . F(5) F 1.3320(18) 0.2028(15) 0.1440(13) 0.152(7) Uiso 0.63(2) 1 d P A 1 F(6) F 1.4707(13) 0.1313(10) 0.0809(9) 0.109(4) Uiso 0.63(2) 1 d P A 1 F(7) F 1.3403(18) 0.1016(14) 0.1650(12) 0.088(6) Uiso 0.37(2) 1 d P A 2 F(8) F 1.4154(19) 0.0851(15) 0.0425(13) 0.094(6) Uiso 0.37(2) 1 d P A 2 O(1) O 1.4247(12) 0.5019(6) 0.0743(5) 0.115(4) Uani 1.00 1 d . . . N(1) N 1.2935(11) 0.3045(9) 0.6124(9) 0.056(3) Uiso 0.64(2) 1 d P B 3 N(2) N 1.3148(15) 0.3361(13) 0.5716(12) 0.040(4) Uiso 0.36(2) 1 d P B 4 C(1) C 1.2148(11) 0.3163(9) 0.5696(9) 0.042(2) Uiso 0.64(2) 1 d P B 3 C(2) C 1.3917(16) 0.2895(12) 0.6697(12) 0.074(4) Uiso 0.64(2) 1 d PD B 3 C(3) C 1.5126(18) 0.2685(18) 0.6210(16) 0.098(6) Uiso 0.64(2) 1 d PD B 3 C(4) C 1.3588(17) 0.3791(12) 0.6898(13) 0.077(4) Uiso 0.64(2) 1 d PD B 3 C(5) C 1.394(2) 0.1997(15) 0.7480(13) 0.091(6) Uiso 0.64(2) 1 d PD B 3 C(6) C 1.1739(6) 0.2973(5) 0.2881(6) 0.0502(18) Uani 1.00 1 d . . . C(7) C 1.0954(6) 0.1578(5) 0.2692(4) 0.0385(13) Uani 1.00 1 d . . . C(8) C 0.8882(5) 0.0065(4) 0.7578(4) 0.0344(12) Uani 1.00 1 d . . . C(11) C 1.0770(7) 0.4990(5) 0.2713(6) 0.054(2) Uani 1.00 1 d . . . C(12) C 1.0126(10) 0.5632(6) 0.3073(7) 0.070(2) Uani 1.00 1 d . . . C(13) C 0.9436(12) 0.6562(7) 0.2557(9) 0.084(3) Uani 1.00 1 d . . . C(14) C 0.9372(10) 0.6833(6) 0.1711(8) 0.072(2) Uani 1.00 1 d . . . C(15) C 1.0064(15) 0.6210(9) 0.1365(8) 0.099(4) Uani 1.00 1 d . . . C(16) C 1.0741(13) 0.5276(7) 0.1831(7) 0.093(4) Uani 1.00 1 d . . . C(17) C 1.3204(9) 0.3867(8) 0.3437(8) 0.075(2) Uani 1.00 1 d . . . C(18) C 1.3344(12) 0.4443(10) 0.3895(11) 0.097(4) Uani 1.00 1 d . . . C(19) C 1.4455(14) 0.4544(12) 0.3952(11) 0.107(4) Uani 1.00 1 d . . . C(20) C 1.5478(15) 0.3978(16) 0.3544(16) 0.143(7) Uani 1.00 1 d . . . C(21) C 1.5321(13) 0.3602(15) 0.3094(14) 0.130(7) Uani 1.00 1 d . . . C(22) C 1.4115(13) 0.3552(14) 0.3081(14) 0.123(6) Uani 1.00 1 d . . . C(23) C 0.9356(7) 0.3563(6) 0.2134(5) 0.0527(19) Uani 1.00 1 d . . . C(24) C 0.8356(10) 0.4206(9) 0.2339(6) 0.094(4) Uani 1.00 1 d . . . C(25) C 0.7597(15) 0.4973(13) 0.1685(9) 0.135(7) Uani 1.00 1 d . . . C(26) C 0.7867(14) 0.5137(10) 0.0862(8) 0.113(5) Uani 1.00 1 d . . . C(27) C 0.8837(14) 0.4516(9) 0.0657(6) 0.093(4) Uani 1.00 1 d . . . C(28) C 0.9575(9) 0.3736(6) 0.1284(5) 0.064(2) Uani 1.00 1 d . . . C(29) C 1.1183(6) -0.1444(5) 0.7953(4) 0.0435(16) Uani 1.00 1 d . . . C(30) C 1.2371(7) -0.1610(7) 0.7680(5) 0.059(2) Uani 1.00 1 d . . . C(31) C 1.3318(8) -0.2079(10) 0.8291(7) 0.086(3) Uani 1.00 1 d . . . C(32) C 1.3086(9) -0.2347(10) 0.9158(7) 0.082(3) Uani 1.00 1 d . . . C(33) C 1.1899(9) -0.2199(8) 0.9433(5) 0.069(2) Uani 1.00 1 d . . . C(34) C 1.0948(7) -0.1757(6) 0.8834(5) 0.0520(19) Uani 1.00 1 d . . . C(35) C 1.0477(6) 0.0843(5) 0.8124(4) 0.0364(13) Uani 1.00 1 d . . . C(36) C 1.1656(7) 0.0551(8) 0.7869(5) 0.066(2) Uani 1.00 1 d . . . C(37) C 1.2621(8) 0.0265(9) 0.8433(6) 0.072(2) Uani 1.00 1 d . . . C(38) C 1.2421(7) 0.0293(6) 0.9234(5) 0.0496(17) Uani 1.00 1 d . . . C(39) C 1.1245(7) 0.0585(5) 0.9490(4) 0.0438(15) Uani 1.00 1 d . . . C(40) C 1.0265(6) 0.0852(5) 0.8946(4) 0.0385(13) Uani 1.00 1 d . . . C(41) C 0.7925(6) 0.1860(5) 0.7817(4) 0.0392(14) Uani 1.00 1 d . . . C(42) C 0.7748(7) 0.2828(5) 0.7588(5) 0.0476(17) Uani 1.00 1 d . . . C(43) C 0.6824(8) 0.3372(6) 0.7967(5) 0.056(2) Uani 1.00 1 d . . . C(44) C 0.6080(7) 0.2936(6) 0.8560(5) 0.052(2) Uani 1.00 1 d . . . C(45) C 0.6253(7) 0.1966(6) 0.8795(5) 0.054(2) Uani 1.00 1 d . . . C(46) C 0.7176(7) 0.1413(6) 0.8420(4) 0.0468(17) Uani 1.00 1 d . . . C(47) C 0.502(2) 0.0417(16) 0.3279(15) 0.079(6) Uani 0.50 1 d P . . C(51) C 1.235(2) 0.3433(17) 0.5363(16) 0.043(4) Uiso 0.36(2) 1 d P B 4 C(52) C 1.419(2) 0.3265(18) 0.6184(17) 0.059(6) Uiso 0.36(2) 1 d PD B 4 C(53) C 1.392(3) 0.412(2) 0.640(2) 0.078(8) Uiso 0.36(2) 1 d PD B 4 C(54) C 1.530(3) 0.312(3) 0.567(2) 0.096(11) Uiso 0.36(2) 1 d PD B 4 C(55) C 1.403(4) 0.255(3) 0.708(2) 0.102(13) Uiso 0.36(2) 1 d PD B 4 H(1) H 1.5453 0.2011 0.6345 0.118 Uiso 0.64(2) 1 c R B 3 H(2) H 1.5691 0.2906 0.6377 0.118 Uiso 0.64(2) 1 c R B 3 H(3) H 1.4973 0.3009 0.5608 0.118 Uiso 0.64(2) 1 c R B 3 H(4) H 1.3932 0.4248 0.6481 0.092 Uiso 0.64(2) 1 c R B 3 H(5) H 1.3896 0.3630 0.7452 0.092 Uiso 0.64(2) 1 c R B 3 H(6) H 1.2729 0.4060 0.6886 0.092 Uiso 0.64(2) 1 c R B 3 H(7) H 1.3416 0.2167 0.7900 0.109 Uiso 0.64(2) 1 c R B 3 H(8) H 1.4749 0.1686 0.7708 0.109 Uiso 0.64(2) 1 c R B 3 H(9) H 1.3683 0.1574 0.7322 0.109 Uiso 0.64(2) 1 c R B 3 H(10) H 1.1863 0.3289 0.2281 0.060 Uiso 1.00 1 c R . . H(11) H 1.2414 0.2410 0.3108 0.060 Uiso 1.00 1 c R . . H(12) H 0.8099 0.0238 0.7325 0.041 Uiso 1.00 1 c R . . H(13) H 0.8838 -0.0259 0.8182 0.041 Uiso 1.00 1 c R . . H(14) H 1.0117 0.5434 0.3687 0.087 Uiso 1.00 1 c R . . H(15) H 0.8993 0.7009 0.2820 0.103 Uiso 1.00 1 c R . . H(16) H 0.8848 0.7458 0.1359 0.084 Uiso 1.00 1 c R . . H(17) H 1.0066 0.6422 0.0732 0.111 Uiso 1.00 1 c R . . H(18) H 1.1195 0.4837 0.1564 0.113 Uiso 1.00 1 c R . . H(19) H 1.2623 0.4790 0.4128 0.112 Uiso 1.00 1 c R . . H(20) H 1.4575 0.4934 0.4223 0.129 Uiso 1.00 1 c R . . H(21) H 1.6290 0.3919 0.3654 0.172 Uiso 1.00 1 c R . . H(22) H 1.5956 0.3352 0.2766 0.156 Uiso 1.00 1 c R . . H(23) H 1.4001 0.3236 0.2697 0.157 Uiso 1.00 1 c R . . H(24) H 0.8168 0.4099 0.2943 0.111 Uiso 1.00 1 c R . . H(25) H 0.6884 0.5381 0.1848 0.152 Uiso 1.00 1 c R . . H(26) H 0.7384 0.5688 0.0390 0.148 Uiso 1.00 1 c R . . H(27) H 0.9037 0.4626 0.0067 0.107 Uiso 1.00 1 c R . . H(28) H 1.0253 0.3302 0.1125 0.077 Uiso 1.00 1 c R . . H(29) H 1.2546 -0.1417 0.7079 0.070 Uiso 1.00 1 c R . . H(30) H 1.4143 -0.2178 0.8087 0.104 Uiso 1.00 1 c R . . H(31) H 1.3746 -0.2595 0.9558 0.100 Uiso 1.00 1 c R . . H(32) H 1.1732 -0.2391 1.0030 0.079 Uiso 1.00 1 c R . . H(33) H 1.0128 -0.1674 0.9021 0.062 Uiso 1.00 1 c R . . H(34) H 1.1818 0.0523 0.7315 0.077 Uiso 1.00 1 c R . . H(35) H 1.3442 0.0053 0.8257 0.084 Uiso 1.00 1 c R . . H(36) H 1.3071 0.0144 0.9605 0.060 Uiso 1.00 1 c R . . H(37) H 1.1102 0.0587 1.0056 0.052 Uiso 1.00 1 c R . . H(38) H 0.9444 0.1054 0.9126 0.045 Uiso 1.00 1 c R . . H(39) H 0.8257 0.3144 0.7164 0.056 Uiso 1.00 1 c R . . H(40) H 0.6723 0.4044 0.7810 0.066 Uiso 1.00 1 c R . . H(41) H 0.5456 0.3310 0.8799 0.061 Uiso 1.00 1 c R . . H(42) H 0.5752 0.1665 0.9216 0.063 Uiso 1.00 1 c R . . H(43) H 0.7275 0.0746 0.8581 0.057 Uiso 1.00 1 c R . . H(44) H 1.1608 0.1117 0.3073 0.048 Uiso 1.00 1 c R . . H(45) H 1.1241 0.1779 0.2124 0.048 Uiso 1.00 1 c R . . H(46) H 0.4781 0.0797 0.2667 0.095 Uiso 0.50 1 c R . . H(47) H 0.5854 -0.0029 0.3300 0.095 Uiso 0.50 1 c R . . H(51) H 1.4187 0.4602 0.5954 0.093 Uiso 0.36(2) 1 c R B 4 H(52) H 1.4337 0.3947 0.6922 0.093 Uiso 0.36(2) 1 c R B 4 H(53) H 1.3073 0.4354 0.6474 0.093 Uiso 0.36(2) 1 c R B 4 H(54) H 1.5680 0.2453 0.5805 0.115 Uiso 0.36(2) 1 c R B 4 H(55) H 1.5852 0.3383 0.5805 0.115 Uiso 0.36(2) 1 c R B 4 H(56) H 1.5097 0.3437 0.5078 0.115 Uiso 0.36(2) 1 c R B 4 H(57) H 1.3547 0.2897 0.7412 0.122 Uiso 0.36(2) 1 c R B 4 H(58) H 1.4799 0.2184 0.7348 0.122 Uiso 0.36(2) 1 c R B 4 H(59) H 1.3630 0.2137 0.7028 0.122 Uiso 0.36(2) 1 c R B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0445(2) 0.0345(2) 0.0635(3) 0.00326(19) -0.0154(2) -0.0278(2) I(2) 0.0277(2) 0.0332(2) 0.0400(2) -0.00469(16) -0.00079(16) -0.01568(18) I(3) 0.0307(2) 0.0348(2) 0.0338(2) -0.01006(16) 0.00501(15) -0.01771(17) Cu(1) 0.0469(5) 0.0551(6) 0.0792(7) -0.0056(4) -0.0240(5) -0.0359(5) Cu(2) 0.0401(4) 0.0459(4) 0.0280(3) -0.0014(3) 0.0006(3) -0.0149(3) Cu(3) 0.0428(4) 0.0389(4) 0.0292(3) -0.0147(3) 0.0039(3) -0.0133(3) Cu(4) 0.0424(4) 0.0404(4) 0.0310(3) -0.0134(3) 0.0080(3) -0.0179(3) Cl(1) 0.052(2) 0.118(5) 0.170(7) -0.017(2) 0.008(3) -0.103(5) Cl(2) 0.072(3) 0.087(4) 0.124(5) -0.017(3) 0.002(3) -0.036(4) P(1) 0.0288(8) 0.0405(10) 0.0972(17) -0.0137(7) -0.0013(9) -0.0226(10) P(2) 0.0291(7) 0.0315(7) 0.0304(7) -0.0075(6) 0.0063(6) -0.0069(6) P(3) 0.0294(7) 0.0393(8) 0.0273(7) -0.0043(6) 0.0016(5) -0.0178(6) P(4) 0.0302(7) 0.0407(8) 0.0277(7) 0.0008(6) -0.0024(6) -0.0182(6) P(11) 0.0382(10) 0.0857(16) 0.0541(12) -0.0226(10) 0.0146(8) -0.0367(11) O(1) 0.221(12) 0.065(4) 0.070(4) -0.037(6) -0.054(6) -0.029(4) C(6) 0.033(3) 0.036(3) 0.070(5) -0.009(2) 0.013(3) -0.013(3) C(7) 0.031(3) 0.042(3) 0.037(3) -0.009(2) 0.007(2) -0.013(2) C(8) 0.031(2) 0.042(3) 0.028(2) -0.003(2) -0.000(2) -0.018(2) C(11) 0.039(3) 0.038(3) 0.084(6) -0.019(3) 0.004(3) -0.016(3) C(12) 0.092(7) 0.037(4) 0.086(7) -0.010(4) -0.031(5) -0.027(4) C(13) 0.097(8) 0.040(4) 0.116(10) -0.010(5) -0.024(7) -0.031(5) C(14) 0.078(6) 0.037(4) 0.088(7) -0.022(4) -0.006(5) -0.004(4) C(15) 0.135(12) 0.060(6) 0.063(6) -0.017(7) 0.016(7) 0.003(5) C(16) 0.121(10) 0.049(5) 0.067(6) -0.012(5) 0.040(6) -0.000(4) C(17) 0.049(5) 0.080(7) 0.089(7) -0.025(4) -0.002(5) -0.020(5) C(18) 0.076(7) 0.098(9) 0.139(12) -0.039(7) -0.007(7) -0.054(9) C(19) 0.101(10) 0.114(11) 0.133(13) -0.054(9) 0.016(9) -0.060(10) C(20) 0.072(9) 0.161(18) 0.18(2) -0.042(10) 0.024(11) -0.053(16) C(21) 0.076(8) 0.211(19) 0.206(19) -0.077(11) 0.050(10) -0.172(18) C(22) 0.064(7) 0.152(15) 0.178(18) -0.041(9) 0.021(9) -0.087(14) C(23) 0.044(4) 0.054(4) 0.036(3) -0.001(3) 0.001(3) -0.003(3) C(24) 0.070(6) 0.090(8) 0.048(5) 0.040(6) 0.002(4) -0.002(5) C(25) 0.100(10) 0.138(13) 0.069(8) 0.061(9) -0.012(7) -0.013(8) C(26) 0.102(10) 0.092(9) 0.066(7) 0.029(7) -0.017(7) 0.011(6) C(27) 0.123(10) 0.076(7) 0.036(4) -0.010(7) -0.005(5) 0.010(4) C(28) 0.069(5) 0.054(4) 0.037(4) -0.004(4) 0.007(3) 0.001(3) C(29) 0.037(3) 0.050(4) 0.040(3) 0.005(3) -0.007(2) -0.025(3) C(30) 0.032(3) 0.086(6) 0.051(4) 0.006(3) -0.004(3) -0.035(4) C(31) 0.038(4) 0.129(10) 0.072(6) 0.013(5) -0.012(4) -0.047(7) C(32) 0.051(5) 0.111(9) 0.069(6) 0.013(5) -0.022(4) -0.042(6) C(33) 0.061(5) 0.086(6) 0.037(4) 0.011(4) -0.015(3) -0.024(4) C(34) 0.044(4) 0.064(5) 0.038(3) 0.001(3) -0.008(3) -0.020(3) C(35) 0.038(3) 0.037(3) 0.031(3) -0.003(2) -0.005(2) -0.015(2) C(36) 0.036(3) 0.109(8) 0.043(4) 0.006(4) -0.006(3) -0.039(5) C(37) 0.037(4) 0.111(8) 0.055(5) 0.004(4) -0.011(3) -0.036(5) C(38) 0.051(4) 0.048(4) 0.044(3) -0.008(3) -0.020(3) -0.011(3) C(39) 0.056(4) 0.044(3) 0.029(3) -0.014(3) -0.010(3) -0.010(2) C(40) 0.045(3) 0.039(3) 0.033(3) -0.010(2) -0.004(2) -0.016(2) C(41) 0.033(3) 0.048(3) 0.030(3) 0.002(2) -0.001(2) -0.020(2) C(42) 0.044(3) 0.046(4) 0.046(4) 0.003(3) 0.001(3) -0.023(3) C(43) 0.057(4) 0.051(4) 0.054(4) 0.000(3) 0.002(3) -0.028(3) C(44) 0.046(4) 0.056(4) 0.040(3) 0.016(3) -0.007(3) -0.025(3) C(45) 0.044(4) 0.061(4) 0.041(3) 0.002(3) 0.006(3) -0.019(3) C(46) 0.041(3) 0.054(4) 0.033(3) -0.000(3) 0.005(2) -0.017(3) C(47) 0.074(13) 0.063(12) 0.065(12) 0.015(10) -0.010(10) -0.012(9) #============================================================================== _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-II #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) Cu(1) 2.6343(11) yes . . I(1) Cu(2) 2.6256(9) yes . . I(1) Cu(3) 2.7144(11) yes . . I(2) Cu(1) 2.9201(12) yes . . I(2) Cu(2) 2.7004(9) yes . . I(2) Cu(3) 2.8247(8) yes . . I(2) Cu(4) 2.7176(11) yes . . I(3) Cu(3) 2.6391(11) yes . . I(3) Cu(4) 2.7598(8) yes . . I(3) Cu(4) 2.6611(10) yes . 2_756 Cu(1) P(1) 2.249(3) yes . . Cu(1) C(1) 1.939(16) yes . . Cu(1) C(51) 1.92(3) yes . . Cu(2) Cu(3) 2.6173(11) yes . . Cu(2) P(4) 2.2295(16) yes . . Cu(3) P(2) 2.2165(19) yes . . Cu(4) P(3) 2.2429(16) yes . . Cl(1) C(47) 1.79(3) yes . . Cl(2) C(47) 1.59(2) yes . . P(1) C(6) 1.833(11) yes . . P(1) C(11) 1.836(7) yes . . P(1) C(17) 1.827(12) yes . . P(2) C(6) 1.851(9) yes . . P(2) C(7) 1.826(8) yes . . P(2) C(23) 1.810(7) yes . . P(3) C(7) 1.839(9) yes . 2_756 P(3) C(8) 1.846(7) yes . . P(3) C(29) 1.815(7) yes . . P(4) C(8) 1.835(8) yes . . P(4) C(35) 1.832(7) yes . . P(4) C(41) 1.826(7) yes . . P(11) F(1) 1.562(17) yes . . P(11) F(2) 1.673(17) yes . . P(11) F(3) 1.559(15) yes . . P(11) F(4) 1.494(13) yes . . P(11) F(5) 1.51(2) yes . . P(11) F(6) 1.501(13) yes . . P(11) F(7) 1.674(17) yes . . P(11) F(8) 1.66(2) yes . . N(1) C(1) 1.15(2) yes . . N(1) C(2) 1.48(2) yes . . N(2) C(51) 1.11(3) yes . . N(2) C(52) 1.46(3) yes . . C(2) C(3) 1.55(2) yes . . C(2) C(4) 1.51(3) yes . . C(2) C(5) 1.51(2) yes . . C(11) C(12) 1.364(15) yes . . C(11) C(16) 1.380(16) yes . . C(12) C(13) 1.401(12) yes . . C(13) C(14) 1.33(2) yes . . C(14) C(15) 1.342(19) yes . . C(15) C(16) 1.380(14) yes . . C(17) C(18) 1.46(2) yes . . C(17) C(22) 1.22(2) yes . . C(18) C(19) 1.37(2) yes . . C(19) C(20) 1.52(2) yes . . C(20) C(21) 1.20(4) yes . . C(21) C(22) 1.43(2) yes . . C(23) C(24) 1.391(14) yes . . C(23) C(28) 1.365(12) yes . . C(24) C(25) 1.398(16) yes . . C(25) C(26) 1.33(2) yes . . C(26) C(27) 1.35(2) yes . . C(27) C(28) 1.372(13) yes . . C(29) C(30) 1.381(10) yes . . C(29) C(34) 1.400(10) yes . . C(30) C(31) 1.400(13) yes . . C(31) C(32) 1.379(17) yes . . C(32) C(33) 1.381(14) yes . . C(33) C(34) 1.391(12) yes . . C(35) C(36) 1.376(10) yes . . C(35) C(40) 1.391(10) yes . . C(36) C(37) 1.395(14) yes . . C(37) C(38) 1.366(15) yes . . C(38) C(39) 1.373(11) yes . . C(39) C(40) 1.394(11) yes . . C(41) C(42) 1.376(12) yes . . C(41) C(46) 1.390(10) yes . . C(42) C(43) 1.411(12) yes . . C(43) C(44) 1.370(12) yes . . C(44) C(45) 1.379(14) yes . . C(45) C(46) 1.414(12) yes . . C(52) C(53) 1.47(5) yes . . C(52) C(54) 1.48(4) yes . . C(52) C(55) 1.53(4) yes . . C(3) H(1) 0.951 no . . C(3) H(2) 0.950 no . . C(3) H(3) 0.951 no . . C(4) H(4) 0.951 no . . C(4) H(5) 0.950 no . . C(4) H(6) 0.950 no . . C(5) H(7) 0.949 no . . C(5) H(8) 0.950 no . . C(5) H(9) 0.950 no . . C(6) H(10) 0.958 no . . C(6) H(11) 0.952 no . . C(7) H(44) 0.953 no . . C(7) H(45) 0.946 no . . C(8) H(12) 0.960 no . . C(8) H(13) 0.950 no . . C(12) H(14) 0.960 no . . C(13) H(15) 0.962 no . . C(14) H(16) 0.968 no . . C(15) H(17) 0.990 no . . C(16) H(18) 0.961 no . . C(18) H(19) 0.980 no . . C(19) H(20) 0.950 no . . C(20) H(21) 0.950 no . . C(21) H(22) 0.950 no . . C(22) H(23) 1.005 no . . C(24) H(24) 0.979 no . . C(25) H(25) 0.962 no . . C(26) H(26) 0.976 no . . C(27) H(27) 0.958 no . . C(28) H(28) 0.956 no . . C(30) H(29) 0.957 no . . C(31) H(30) 0.967 no . . C(32) H(31) 0.957 no . . C(33) H(32) 0.951 no . . C(34) H(33) 0.953 no . . C(36) H(34) 0.951 no . . C(37) H(35) 0.959 no . . C(38) H(36) 0.947 no . . C(39) H(37) 0.955 no . . C(40) H(38) 0.960 no . . C(42) H(39) 0.965 no . . C(43) H(40) 0.962 no . . C(44) H(41) 0.941 no . . C(45) H(42) 0.946 no . . C(46) H(43) 0.953 no . . C(47) H(46) 0.990 no . . C(47) H(47) 0.990 no . . C(53) H(51) 0.950 no . . C(53) H(52) 0.950 no . . C(53) H(53) 0.949 no . . C(54) H(54) 0.949 no . . C(54) H(55) 0.960 no . . C(54) H(56) 0.950 no . . C(55) H(57) 0.951 no . . C(55) H(58) 0.948 no . . C(55) H(59) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cu(1) I(1) Cu(2) 74.51(3) yes . . . Cu(1) I(1) Cu(3) 66.80(4) yes . . . Cu(2) I(1) Cu(3) 58.67(2) yes . . . Cu(1) I(2) Cu(2) 68.88(3) yes . . . Cu(1) I(2) Cu(3) 61.65(3) yes . . . Cu(1) I(2) Cu(4) 132.55(3) yes . . . Cu(2) I(2) Cu(3) 56.50(2) yes . . . Cu(2) I(2) Cu(4) 68.40(3) yes . . . Cu(3) I(2) Cu(4) 77.97(2) yes . . . Cu(3) I(3) Cu(4) 80.45(2) yes . . . Cu(3) I(3) Cu(4) 89.45(3) yes . . 2_756 Cu(4) I(3) Cu(4) 64.02(2) yes . . 2_756 I(1) Cu(1) I(2) 100.74(4) yes . . . I(1) Cu(1) P(1) 113.52(6) yes . . . I(1) Cu(1) C(1) 118.6(3) yes . . . I(1) Cu(1) C(51) 129.7(7) yes . . . I(2) Cu(1) P(1) 103.96(8) yes . . . I(2) Cu(1) C(1) 92.8(4) yes . . . I(2) Cu(1) C(51) 103.4(6) yes . . . P(1) Cu(1) C(1) 120.6(3) yes . . . P(1) Cu(1) C(51) 102.4(7) yes . . . I(1) Cu(2) I(2) 107.01(3) yes . . . I(1) Cu(2) Cu(3) 62.36(2) yes . . . I(1) Cu(2) P(4) 125.67(6) yes . . . I(2) Cu(2) Cu(3) 64.15(2) yes . . . I(2) Cu(2) P(4) 121.97(5) yes . . . Cu(3) Cu(2) P(4) 159.80(8) yes . . . I(1) Cu(3) I(2) 101.24(3) yes . . . I(1) Cu(3) I(3) 102.31(3) yes . . . I(1) Cu(3) Cu(2) 58.97(3) yes . . . I(1) Cu(3) P(2) 124.49(6) yes . . . I(2) Cu(3) I(3) 100.03(2) yes . . . I(2) Cu(3) Cu(2) 59.35(2) yes . . . I(2) Cu(3) P(2) 102.00(5) yes . . . I(3) Cu(3) Cu(2) 71.69(3) yes . . . I(3) Cu(3) P(2) 121.94(7) yes . . . Cu(2) Cu(3) P(2) 160.10(6) yes . . . I(2) Cu(4) I(3) 99.75(2) yes . . . I(2) Cu(4) I(3) 98.54(3) yes . . 2_756 I(2) Cu(4) P(3) 122.15(7) yes . . . I(3) Cu(4) I(3) 115.98(3) yes . . 2_756 I(3) Cu(4) P(3) 103.38(5) yes . . . I(3) Cu(4) P(3) 116.58(5) yes 2_756 . . Cu(1) P(1) C(6) 114.3(2) yes . . . Cu(1) P(1) C(11) 117.1(3) yes . . . Cu(1) P(1) C(17) 105.2(4) yes . . . C(6) P(1) C(11) 106.2(4) yes . . . C(6) P(1) C(17) 108.0(5) yes . . . C(11) P(1) C(17) 105.4(4) yes . . . Cu(3) P(2) C(6) 110.4(3) yes . . . Cu(3) P(2) C(7) 116.9(2) yes . . . Cu(3) P(2) C(23) 117.8(2) yes . . . C(6) P(2) C(7) 98.4(3) yes . . . C(6) P(2) C(23) 104.0(3) yes . . . C(7) P(2) C(23) 106.9(4) yes . . . Cu(4) P(3) C(7) 115.1(2) yes . . 2_756 Cu(4) P(3) C(8) 112.98(19) yes . . . Cu(4) P(3) C(29) 118.7(2) yes . . . C(7) P(3) C(8) 97.2(3) yes 2_756 . . C(7) P(3) C(29) 106.2(3) yes 2_756 . . C(8) P(3) C(29) 104.2(3) yes . . . Cu(2) P(4) C(8) 110.5(2) yes . . . Cu(2) P(4) C(35) 114.4(2) yes . . . Cu(2) P(4) C(41) 117.89(19) yes . . . C(8) P(4) C(35) 105.8(3) yes . . . C(8) P(4) C(41) 103.4(3) yes . . . C(35) P(4) C(41) 103.6(3) yes . . . F(1) P(11) F(2) 157.3(6) yes . . . F(1) P(11) F(3) 79.8(9) yes . . . F(1) P(11) F(4) 91.1(8) yes . . . F(1) P(11) F(5) 102.9(10) yes . . . F(1) P(11) F(6) 124.2(8) yes . . . F(1) P(11) F(7) 66.6(10) yes . . . F(1) P(11) F(8) 79.3(10) yes . . . F(2) P(11) F(3) 85.0(8) yes . . . F(2) P(11) F(4) 72.4(8) yes . . . F(2) P(11) F(5) 86.9(11) yes . . . F(2) P(11) F(6) 75.8(7) yes . . . F(2) P(11) F(7) 133.6(11) yes . . . F(2) P(11) F(8) 109.6(9) yes . . . F(3) P(11) F(4) 91.3(7) yes . . . F(3) P(11) F(5) 68.9(9) yes . . . F(3) P(11) F(6) 151.1(11) yes . . . F(3) P(11) F(7) 101.4(8) yes . . . F(3) P(11) F(8) 154.0(12) yes . . . F(4) P(11) F(5) 152.8(9) yes . . . F(4) P(11) F(6) 103.0(7) yes . . . F(4) P(11) F(7) 151.4(11) yes . . . F(4) P(11) F(8) 73.8(8) yes . . . F(5) P(11) F(6) 88.4(10) yes . . . F(7) P(11) F(8) 84.2(10) yes . . . C(1) N(1) C(2) 178.1(16) yes . . . C(51) N(2) C(52) 180(2) yes . . . Cu(1) C(1) N(1) 166.4(13) yes . . . N(1) C(2) C(3) 106.4(18) yes . . . N(1) C(2) C(4) 106.1(13) yes . . . N(1) C(2) C(5) 106.7(17) yes . . . C(3) C(2) C(4) 115.8(19) yes . . . C(3) C(2) C(5) 108.1(14) yes . . . C(4) C(2) C(5) 113.2(18) yes . . . P(1) C(6) P(2) 113.4(4) yes . . . P(2) C(7) P(3) 118.9(3) yes . . 2_756 P(3) C(8) P(4) 115.7(3) yes . . . P(1) C(11) C(12) 118.5(7) yes . . . P(1) C(11) C(16) 122.6(7) yes . . . C(12) C(11) C(16) 118.9(7) yes . . . C(11) C(12) C(13) 120.6(11) yes . . . C(12) C(13) C(14) 120.9(12) yes . . . C(13) C(14) C(15) 117.5(9) yes . . . C(14) C(15) C(16) 124.6(12) yes . . . C(11) C(16) C(15) 117.2(11) yes . . . P(1) C(17) C(18) 115.7(8) yes . . . P(1) C(17) C(22) 129.2(17) yes . . . C(18) C(17) C(22) 115.0(16) yes . . . C(17) C(18) C(19) 120.6(14) yes . . . C(18) C(19) C(20) 114(2) yes . . . C(19) C(20) C(21) 123.8(18) yes . . . C(20) C(21) C(22) 116(2) yes . . . C(17) C(22) C(21) 130(2) yes . . . P(2) C(23) C(24) 117.8(6) yes . . . P(2) C(23) C(28) 124.6(6) yes . . . C(24) C(23) C(28) 117.5(7) yes . . . C(23) C(24) C(25) 119.9(11) yes . . . C(24) C(25) C(26) 120.7(14) yes . . . C(25) C(26) C(27) 119.7(11) yes . . . C(26) C(27) C(28) 120.9(10) yes . . . C(23) C(28) C(27) 121.2(9) yes . . . P(3) C(29) C(30) 118.2(5) yes . . . P(3) C(29) C(34) 122.2(5) yes . . . C(30) C(29) C(34) 119.5(7) yes . . . C(29) C(30) C(31) 119.2(8) yes . . . C(30) C(31) C(32) 121.3(9) yes . . . C(31) C(32) C(33) 119.5(9) yes . . . C(32) C(33) C(34) 119.8(8) yes . . . C(29) C(34) C(33) 120.5(7) yes . . . P(4) C(35) C(36) 118.9(6) yes . . . P(4) C(35) C(40) 122.0(5) yes . . . C(36) C(35) C(40) 119.1(7) yes . . . C(35) C(36) C(37) 120.1(9) yes . . . C(36) C(37) C(38) 121.1(8) yes . . . C(37) C(38) C(39) 118.9(8) yes . . . C(38) C(39) C(40) 121.0(7) yes . . . C(35) C(40) C(39) 119.8(6) yes . . . P(4) C(41) C(42) 118.2(5) yes . . . P(4) C(41) C(46) 121.9(6) yes . . . C(42) C(41) C(46) 119.7(7) yes . . . C(41) C(42) C(43) 120.9(7) yes . . . C(42) C(43) C(44) 119.7(8) yes . . . C(43) C(44) C(45) 119.8(8) yes . . . C(44) C(45) C(46) 121.0(7) yes . . . C(41) C(46) C(45) 118.8(8) yes . . . Cl(1) C(47) Cl(2) 112.1(14) yes . . . Cu(1) C(51) N(2) 168(2) yes . . . N(2) C(52) C(53) 108(2) yes . . . N(2) C(52) C(54) 110(2) yes . . . N(2) C(52) C(55) 102(3) yes . . . C(53) C(52) C(54) 113(3) yes . . . C(53) C(52) C(55) 98(3) yes . . . C(54) C(52) C(55) 124(3) yes . . . C(2) C(3) H(1) 109.5 no . . . C(2) C(3) H(2) 109.5 no . . . C(2) C(3) H(3) 109.5 no . . . H(1) C(3) H(2) 109.5 no . . . H(1) C(3) H(3) 109.4 no . . . H(2) C(3) H(3) 109.4 no . . . C(2) C(4) H(4) 109.5 no . . . C(2) C(4) H(5) 109.5 no . . . C(2) C(4) H(6) 109.5 no . . . H(4) C(4) H(5) 109.5 no . . . H(4) C(4) H(6) 109.4 no . . . H(5) C(4) H(6) 109.5 no . . . C(2) C(5) H(7) 109.5 no . . . C(2) C(5) H(8) 109.4 no . . . C(2) C(5) H(9) 109.4 no . . . H(7) C(5) H(8) 109.5 no . . . H(7) C(5) H(9) 109.5 no . . . H(8) C(5) H(9) 109.5 no . . . P(1) C(6) H(10) 108.5 no . . . P(1) C(6) H(11) 108.8 no . . . P(2) C(6) H(10) 108.6 no . . . P(2) C(6) H(11) 108.9 no . . . H(10) C(6) H(11) 108.6 no . . . P(2) C(7) H(44) 109.3 no . . . P(2) C(7) H(45) 109.6 no . . . P(3) C(7) H(44) 97.5 no 2_756 . . P(3) C(7) H(45) 111.3 no 2_756 . . H(44) C(7) H(45) 109.5 no . . . P(3) C(8) H(12) 107.9 no . . . P(3) C(8) H(13) 108.3 no . . . P(4) C(8) H(12) 107.8 no . . . P(4) C(8) H(13) 108.3 no . . . H(12) C(8) H(13) 108.6 no . . . C(11) C(12) H(14) 119.6 no . . . C(13) C(12) H(14) 119.8 no . . . C(12) C(13) H(15) 119.6 no . . . C(14) C(13) H(15) 119.4 no . . . C(13) C(14) H(16) 121.0 no . . . C(15) C(14) H(16) 121.4 no . . . C(14) C(15) H(17) 118.1 no . . . C(16) C(15) H(17) 117.2 no . . . C(11) C(16) H(18) 120.2 no . . . C(15) C(16) H(18) 122.6 no . . . C(17) C(18) H(19) 119.1 no . . . C(19) C(18) H(19) 120.2 no . . . C(18) C(19) H(20) 123.0 no . . . C(20) C(19) H(20) 123.0 no . . . C(19) C(20) H(21) 118.1 no . . . C(21) C(20) H(21) 118.1 no . . . C(20) C(21) H(22) 122.1 no . . . C(22) C(21) H(22) 122.1 no . . . C(17) C(22) H(23) 115.7 no . . . C(21) C(22) H(23) 114.5 no . . . C(23) C(24) H(24) 119.6 no . . . C(25) C(24) H(24) 120.5 no . . . C(24) C(25) H(25) 117.9 no . . . C(26) C(25) H(25) 121.4 no . . . C(25) C(26) H(26) 122.9 no . . . C(27) C(26) H(26) 117.4 no . . . C(26) C(27) H(27) 120.3 no . . . C(28) C(27) H(27) 118.7 no . . . C(23) C(28) H(28) 119.1 no . . . C(27) C(28) H(28) 119.7 no . . . C(29) C(30) H(29) 120.5 no . . . C(31) C(30) H(29) 120.3 no . . . C(30) C(31) H(30) 117.9 no . . . C(32) C(31) H(30) 120.7 no . . . C(31) C(32) H(31) 119.6 no . . . C(33) C(32) H(31) 120.8 no . . . C(32) C(33) H(32) 120.1 no . . . C(34) C(33) H(32) 120.1 no . . . C(29) C(34) H(33) 119.3 no . . . C(33) C(34) H(33) 120.2 no . . . C(35) C(36) H(34) 120.3 no . . . C(37) C(36) H(34) 119.6 no . . . C(36) C(37) H(35) 120.0 no . . . C(38) C(37) H(35) 118.8 no . . . C(37) C(38) H(36) 121.7 no . . . C(39) C(38) H(36) 119.4 no . . . C(38) C(39) H(37) 119.1 no . . . C(40) C(39) H(37) 119.9 no . . . C(35) C(40) H(38) 119.3 no . . . C(39) C(40) H(38) 121.0 no . . . C(41) C(42) H(39) 120.1 no . . . C(43) C(42) H(39) 119.0 no . . . C(42) C(43) H(40) 119.9 no . . . C(44) C(43) H(40) 120.4 no . . . C(43) C(44) H(41) 118.9 no . . . C(45) C(44) H(41) 121.3 no . . . C(44) C(45) H(42) 119.5 no . . . C(46) C(45) H(42) 119.5 no . . . C(41) C(46) H(43) 121.1 no . . . C(45) C(46) H(43) 120.1 no . . . Cl(1) C(47) H(46) 109.2 no . . . Cl(1) C(47) H(47) 109.2 no . . . Cl(2) C(47) H(46) 109.2 no . . . Cl(2) C(47) H(47) 109.2 no . . . H(46) C(47) H(47) 107.9 no . . . C(52) C(53) H(51) 109.5 no . . . C(52) C(53) H(52) 109.5 no . . . C(52) C(53) H(53) 109.6 no . . . H(51) C(53) H(52) 109.4 no . . . H(51) C(53) H(53) 109.4 no . . . H(52) C(53) H(53) 109.4 no . . . C(52) C(54) H(54) 109.5 no . . . C(52) C(54) H(55) 109.6 no . . . C(52) C(54) H(56) 109.5 no . . . H(54) C(54) H(55) 109.5 no . . . H(54) C(54) H(56) 109.4 no . . . H(55) C(54) H(56) 109.4 no . . . C(52) C(55) H(57) 109.4 no . . . C(52) C(55) H(58) 109.5 no . . . C(52) C(55) H(59) 109.4 no . . . H(57) C(55) H(58) 109.5 no . . . H(57) C(55) H(59) 109.4 no . . . H(58) C(55) H(59) 109.6 no . . . #============================================================================== #============================================================================== # End of CIF #============================================================================== #==============================================================================