Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Maravanji Balakrishna' _publ_contact_author_email KRISHNA@CHEM.IITB.AC.IN _publ_section_title ; Novel Octanuclear Copper(I) Metallomacrocycles and Their Transformation into Hexanuclear 2-Dimensional Grids of Copper(I) Coordination Polymers Containing Cyclodiphosphazanes, [(?-NtBuP)2(C4H8X)2] (X = NMe, O) ; loop_ _publ_author_name 'Maravanji Balakrishna' 'Joel Mague' 'D. Suresh' # Attachment 'Compound_3.cif' data_msb347 _database_code_depnum_ccdc_archive 'CCDC 678205' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H88 Cl2 Cu4 I4 N14 P4' _chemical_formula_sum 'C41 H88 Cl2 Cu4 I4 N14 P4' _chemical_formula_weight 1733.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2608(8) _cell_length_b 18.556(1) _cell_length_c 18.541(1) _cell_angle_alpha 68.787(1) _cell_angle_beta 80.755(1) _cell_angle_gamma 81.243(1) _cell_volume 3231.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3010 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 28.32 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 3.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6003 _exptl_absorpt_correction_T_max 0.7476 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2005a)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 deg. in omega, colllected at phi = 0.00, 90.00 and 180.00 deg. and 2 sets of 800 frames, each of width 0.45 deg in phi, collected at omega = -30.00 and 210.00 deg. From an inspection of a reciprocal space plot prepared from 2404 reflections harvested from the full data set it was evident that the crystal contained two components. Two orientations of a triclinic unit cell differing by a 5.2 deg. rotation about {1,0,0.45} were obtained from CELL_NOW (Sheldrick, 2005) and these orientation matrices were used in the multicomponent version of SAINT+ to integrate the reflections from the two domains. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXSW Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35593 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.37 _reflns_number_total 31619 _reflns_number_gt 22691 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2005). CELL_NOW. University of G\"ottingen, Germany. Sheldrick, G, M. (2005a). TWINABS, Version 1.02. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.98 - 0.99 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31619 _refine_ls_number_parameters 641 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 I1 I 0.713696(19) 0.745070(12) 1.044670(11) 0.02057(5) Uani 1 1 d . . . I2 I 1.071305(19) 0.698297(12) 0.935019(11) 0.01957(5) Uani 1 1 d . . . I3 I 0.974987(19) 0.636558(11) 0.599285(11) 0.01932(5) Uani 1 1 d . . . I4 I 0.588570(19) 0.594607(11) 0.698877(12) 0.01921(5) Uani 1 1 d . . . Cu1 Cu 0.94941(3) 0.66650(2) 1.08338(2) 0.01598(8) Uani 1 1 d . . . Cu2 Cu 0.83924(3) 0.76994(2) 0.90864(2) 0.01526(8) Uani 1 1 d . . . Cu3 Cu 0.78963(3) 0.671519(19) 0.70571(2) 0.01427(7) Uani 1 1 d . . . Cu4 Cu 0.82734(3) 0.529787(19) 0.68013(2) 0.01550(8) Uani 1 1 d . . . P1 P 1.03456(7) 0.69908(4) 1.16874(4) 0.01202(14) Uani 1 1 d . . . P2 P 0.75931(7) 0.84606(4) 0.79980(4) 0.01184(14) Uani 1 1 d . . . P3 P 0.73582(7) 0.79722(4) 0.69001(4) 0.01141(14) Uani 1 1 d . . . P4 P 0.85710(7) 0.40188(4) 0.71472(4) 0.01152(14) Uani 1 1 d . . . N1 N 1.1906(2) 0.65794(13) 1.19412(13) 0.0112(5) Uani 1 1 d . . . N2 N 1.0160(2) 0.79403(13) 1.15188(13) 0.0140(5) Uani 1 1 d . . . N3 N 0.9406(2) 0.95656(13) 1.12195(14) 0.0154(5) Uani 1 1 d . . . N4 N 0.9099(2) 0.55425(14) 1.12346(14) 0.0194(5) Uani 1 1 d . . . N5 N 0.7201(2) 0.93477(13) 0.80334(14) 0.0145(5) Uani 1 1 d . . . N6 N 0.6214(2) 1.07806(14) 0.82673(16) 0.0228(6) Uani 1 1 d . . . N7 N 0.8397(2) 0.84985(13) 0.71004(13) 0.0119(5) Uani 1 1 d . . . N8 N 0.6363(2) 0.82073(13) 0.76513(13) 0.0114(5) Uani 1 1 d . . . N9 N 0.6871(2) 0.84825(13) 0.60314(13) 0.0134(5) Uani 1 1 d . . . N10 N 0.6375(2) 0.92440(13) 0.44388(13) 0.0160(5) Uani 1 1 d . . . N11 N 0.8409(2) 0.61107(14) 0.81427(15) 0.0181(5) Uani 1 1 d . . . N12 N 1.0060(2) 0.34523(13) 0.73380(13) 0.0120(5) Uani 1 1 d . . . N13 N 0.7808(2) 0.38001(13) 0.65382(13) 0.0124(5) Uani 1 1 d . . . N14 N 0.6311(2) 0.35305(14) 0.55129(14) 0.0167(5) Uani 1 1 d . . . C1 C 1.3113(3) 0.64992(16) 1.14002(16) 0.0144(6) Uani 1 1 d . . . C2 C 1.3172(3) 0.72749(17) 1.07279(17) 0.0203(6) Uani 1 1 d . . . H2A H 1.2392 0.7378 1.0448 0.030 Uiso 1 1 calc R . . H2B H 1.3980 0.7253 1.0371 0.030 Uiso 1 1 calc R . . H2C H 1.3180 0.7692 1.0934 0.030 Uiso 1 1 calc R . . C3 C 1.3049(3) 0.58433(17) 1.10911(17) 0.0186(6) Uani 1 1 d . . . H3A H 1.3057 0.5345 1.1524 0.028 Uiso 1 1 calc R . . H3B H 1.3817 0.5828 1.0706 0.028 Uiso 1 1 calc R . . H3C H 1.2231 0.5937 1.0847 0.028 Uiso 1 1 calc R . . C4 C 1.4338(3) 0.63256(17) 1.18346(17) 0.0193(6) Uani 1 1 d . . . H4A H 1.4424 0.6769 1.1986 0.029 Uiso 1 1 calc R . . H4B H 1.5132 0.6235 1.1494 0.029 Uiso 1 1 calc R . . H4C H 1.4241 0.5861 1.2302 0.029 Uiso 1 1 calc R . . C5 C 1.0473(3) 0.83104(16) 1.20332(17) 0.0171(6) Uani 1 1 d . . . H5A H 1.1376 0.8481 1.1865 0.021 Uiso 1 1 calc R . . H5B H 1.0456 0.7933 1.2572 0.021 Uiso 1 1 calc R . . C6 C 0.9467(3) 0.90081(16) 1.20140(17) 0.0172(6) Uani 1 1 d . . . H6A H 0.8580 0.8828 1.2230 0.021 Uiso 1 1 calc R . . H6B H 0.9713 0.9269 1.2346 0.021 Uiso 1 1 calc R . . C7 C 1.0078(3) 0.84913(16) 1.07228(16) 0.0155(6) Uani 1 1 d . . . H7A H 0.9822 0.8227 1.0396 0.019 Uiso 1 1 calc R . . H7B H 1.0957 0.8679 1.0496 0.019 Uiso 1 1 calc R . . C8 C 0.9064(3) 0.91728(16) 1.07267(17) 0.0171(6) Uani 1 1 d . . . H8A H 0.9029 0.9545 1.0188 0.021 Uiso 1 1 calc R . . H8B H 0.8176 0.8988 1.0924 0.021 Uiso 1 1 calc R . . C9 C 0.8415(3) 1.02110(17) 1.12392(19) 0.0221(7) Uani 1 1 d . . . H9A H 0.8349 1.0579 1.0708 0.033 Uiso 1 1 calc R . . H9B H 0.8677 1.0475 1.1558 0.033 Uiso 1 1 calc R . . H9C H 0.7553 1.0014 1.1465 0.033 Uiso 1 1 calc R . . C10 C 0.8660(3) 0.49783(17) 1.16103(17) 0.0187(6) Uani 1 1 d . . . C11 C 0.8085(3) 0.42664(17) 1.21105(19) 0.0256(7) Uani 1 1 d . . . H11A H 0.7133 0.4386 1.2243 0.038 Uiso 1 1 calc R . . H11B H 0.8519 0.4042 1.2588 0.038 Uiso 1 1 calc R . . H11C H 0.8216 0.3894 1.1836 0.038 Uiso 1 1 calc R . . C12 C 0.7708(3) 0.95822(17) 0.85974(18) 0.0182(6) Uani 1 1 d . . . H12A H 0.8494 0.9868 0.8347 0.022 Uiso 1 1 calc R . . H12B H 0.7986 0.9115 0.9034 0.022 Uiso 1 1 calc R . . C13 C 0.6649(3) 1.00950(18) 0.89054(19) 0.0236(7) Uani 1 1 d . . . H13A H 0.5883 0.9799 0.9182 0.028 Uiso 1 1 calc R . . H13B H 0.7008 1.0257 0.9282 0.028 Uiso 1 1 calc R . . C14 C 0.5679(3) 1.05415(17) 0.77176(19) 0.0225(7) Uani 1 1 d . . . H14A H 0.5391 1.1009 0.7284 0.027 Uiso 1 1 calc R . . H14B H 0.4891 1.0262 0.7982 0.027 Uiso 1 1 calc R . . C15 C 0.6691(3) 1.00191(16) 0.73923(18) 0.0200(6) Uani 1 1 d . . . H15A H 0.6274 0.9836 0.7053 0.024 Uiso 1 1 calc R . . H15B H 0.7434 1.0315 0.7073 0.024 Uiso 1 1 calc R . . C16 C 0.5208(3) 1.1283(2) 0.8564(2) 0.0361(9) Uani 1 1 d . . . H16A H 0.4445 1.0995 0.8841 0.054 Uiso 1 1 calc R . . H16B H 0.4920 1.1738 0.8129 0.054 Uiso 1 1 calc R . . H16C H 0.5584 1.1452 0.8923 0.054 Uiso 1 1 calc R . . C17 C 0.9836(3) 0.85884(16) 0.68220(16) 0.0139(6) Uani 1 1 d . . . C18 C 1.0657(3) 0.77984(16) 0.69974(17) 0.0181(6) Uani 1 1 d . . . H18A H 1.0537 0.7509 0.7559 0.027 Uiso 1 1 calc R . . H18B H 1.1598 0.7874 0.6829 0.027 Uiso 1 1 calc R . . H18C H 1.0365 0.7505 0.6717 0.027 Uiso 1 1 calc R . . C19 C 0.9959(3) 0.90427(18) 0.59495(17) 0.0213(7) Uani 1 1 d . . . H19A H 0.9596 0.8762 0.5682 0.032 Uiso 1 1 calc R . . H19B H 1.0896 0.9101 0.5752 0.032 Uiso 1 1 calc R . . H19C H 0.9463 0.9557 0.5853 0.032 Uiso 1 1 calc R . . C20 C 1.0316(3) 0.90543(17) 0.72416(18) 0.0204(7) Uani 1 1 d . . . H20A H 0.9782 0.9559 0.7134 0.031 Uiso 1 1 calc R . . H20B H 1.1250 0.9135 0.7056 0.031 Uiso 1 1 calc R . . H20C H 1.0223 0.8768 0.7804 0.031 Uiso 1 1 calc R . . C21 C 0.5101(3) 0.78917(16) 0.80812(16) 0.0145(6) Uani 1 1 d . . . C22 C 0.5332(3) 0.70617(16) 0.86541(17) 0.0172(6) Uani 1 1 d . . . H22A H 0.5756 0.6719 0.8368 0.026 Uiso 1 1 calc R . . H22B H 0.4479 0.6882 0.8930 0.026 Uiso 1 1 calc R . . H22C H 0.5909 0.7053 0.9031 0.026 Uiso 1 1 calc R . . C23 C 0.4406(3) 0.84245(17) 0.85210(18) 0.0200(6) Uani 1 1 d . . . H23A H 0.4972 0.8430 0.8897 0.030 Uiso 1 1 calc R . . H23B H 0.3561 0.8233 0.8798 0.030 Uiso 1 1 calc R . . H23C H 0.4239 0.8953 0.8151 0.030 Uiso 1 1 calc R . . C24 C 0.4225(3) 0.79010(17) 0.74804(17) 0.0187(6) Uani 1 1 d . . . H24A H 0.4079 0.8432 0.7112 0.028 Uiso 1 1 calc R . . H24B H 0.3369 0.7718 0.7748 0.028 Uiso 1 1 calc R . . H24C H 0.4666 0.7559 0.7198 0.028 Uiso 1 1 calc R . . C25 C 0.6540(3) 0.93246(16) 0.57227(17) 0.0173(6) Uani 1 1 d . . . H25A H 0.6998 0.9576 0.5986 0.021 Uiso 1 1 calc R . . H25B H 0.5571 0.9451 0.5828 0.021 Uiso 1 1 calc R . . C26 C 0.6961(3) 0.96344(16) 0.48499(17) 0.0180(6) Uani 1 1 d . . . H26A H 0.6683 1.0199 0.4644 0.022 Uiso 1 1 calc R . . H26B H 0.7940 0.9558 0.4752 0.022 Uiso 1 1 calc R . . C27 C 0.6796(3) 0.84083(16) 0.47461(17) 0.0178(6) Uani 1 1 d . . . H27A H 0.7775 0.8319 0.4657 0.021 Uiso 1 1 calc R . . H27B H 0.6414 0.8139 0.4468 0.021 Uiso 1 1 calc R . . C28 C 0.6342(3) 0.80784(17) 0.56081(17) 0.0181(6) Uani 1 1 d . . . H28A H 0.5360 0.8136 0.5694 0.022 Uiso 1 1 calc R . . H28B H 0.6651 0.7517 0.5810 0.022 Uiso 1 1 calc R . . C29 C 0.6787(3) 0.95509(18) 0.36059(17) 0.0219(7) Uani 1 1 d . . . H29A H 0.6523 1.0112 0.3407 0.033 Uiso 1 1 calc R . . H29B H 0.6363 0.9294 0.3341 0.033 Uiso 1 1 calc R . . H29C H 0.7754 0.9454 0.3508 0.033 Uiso 1 1 calc R . . C30 C 0.8306(3) 0.58214(17) 0.87941(18) 0.0188(6) Uani 1 1 d . . . C31 C 0.8126(3) 0.54527(19) 0.96452(18) 0.0288(8) Uani 1 1 d . . . H31A H 0.8407 0.5787 0.9885 0.043 Uiso 1 1 calc R . . H31B H 0.8664 0.4949 0.9797 0.043 Uiso 1 1 calc R . . H31C H 0.7189 0.5376 0.9822 0.043 Uiso 1 1 calc R . . C32 C 1.1375(3) 0.35761(16) 0.68683(16) 0.0143(6) Uani 1 1 d . . . C33 C 1.2076(3) 0.41606(17) 0.70427(18) 0.0215(7) Uani 1 1 d . . . H33A H 1.1512 0.4655 0.6940 0.032 Uiso 1 1 calc R . . H33B H 1.2923 0.4244 0.6709 0.032 Uiso 1 1 calc R . . H33C H 1.2241 0.3955 0.7590 0.032 Uiso 1 1 calc R . . C34 C 1.2234(3) 0.28013(17) 0.70480(18) 0.0229(7) Uani 1 1 d . . . H34A H 1.2294 0.2573 0.7610 0.034 Uiso 1 1 calc R . . H34B H 1.3125 0.2884 0.6769 0.034 Uiso 1 1 calc R . . H34C H 1.1837 0.2448 0.6881 0.034 Uiso 1 1 calc R . . C35 C 1.1144(3) 0.38877(18) 0.60107(16) 0.0212(7) Uani 1 1 d . . . H35A H 1.0653 0.3528 0.5907 0.032 Uiso 1 1 calc R . . H35B H 1.2000 0.3936 0.5685 0.032 Uiso 1 1 calc R . . H35C H 1.0628 0.4399 0.5890 0.032 Uiso 1 1 calc R . . C36 C 0.7800(3) 0.43251(16) 0.57251(16) 0.0150(6) Uani 1 1 d . . . H36A H 0.8559 0.4157 0.5399 0.018 Uiso 1 1 calc R . . H36B H 0.7902 0.4859 0.5690 0.018 Uiso 1 1 calc R . . C37 C 0.6515(3) 0.43218(16) 0.54240(17) 0.0177(6) Uani 1 1 d . . . H37A H 0.5764 0.4539 0.5717 0.021 Uiso 1 1 calc R . . H37B H 0.6544 0.4653 0.4868 0.021 Uiso 1 1 calc R . . C38 C 0.6231(3) 0.30477(16) 0.63394(17) 0.0170(6) Uani 1 1 d . . . H38A H 0.6053 0.2517 0.6405 0.020 Uiso 1 1 calc R . . H38B H 0.5492 0.3269 0.6636 0.020 Uiso 1 1 calc R . . C39 C 0.7526(3) 0.30133(16) 0.66502(17) 0.0159(6) Uani 1 1 d . . . H39A H 0.7465 0.2696 0.7211 0.019 Uiso 1 1 calc R . . H39B H 0.8256 0.2765 0.6374 0.019 Uiso 1 1 calc R . . C40 C 0.5110(3) 0.35352(19) 0.51732(19) 0.0262(7) Uani 1 1 d . . . H40A H 0.5006 0.3005 0.5214 0.039 Uiso 1 1 calc R . . H40B H 0.5190 0.3869 0.4624 0.039 Uiso 1 1 calc R . . H40C H 0.4334 0.3734 0.5455 0.039 Uiso 1 1 calc R . . C41 C 0.1902(4) 0.8024(2) 0.4790(2) 0.0343(9) Uani 1 1 d . . . H41A H 0.1453 0.7926 0.5326 0.041 Uiso 1 1 calc R . . H41B H 0.2229 0.7516 0.4732 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.32415(9) 0.85610(5) 0.46422(6) 0.0398(2) Uani 1 1 d . . . Cl2 Cl 0.07369(9) 0.85418(6) 0.40993(6) 0.0388(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.01653(9) 0.02722(11) 0.01623(10) -0.00550(8) -0.00166(8) -0.00238(8) I2 0.01856(10) 0.02531(10) 0.01351(10) -0.00609(8) -0.00420(7) 0.00267(8) I3 0.02448(10) 0.01678(9) 0.01727(10) -0.00782(8) 0.00478(8) -0.00649(8) I4 0.01931(10) 0.01639(9) 0.02225(11) -0.00584(8) -0.00543(8) -0.00169(8) Cu1 0.01909(18) 0.01670(18) 0.01329(18) -0.00498(15) -0.00500(14) -0.00242(15) Cu2 0.01724(17) 0.01544(17) 0.01337(18) -0.00434(14) -0.00486(14) -0.00083(14) Cu3 0.01764(17) 0.01157(16) 0.01368(18) -0.00427(14) -0.00342(14) -0.00021(14) Cu4 0.01952(18) 0.01202(17) 0.01468(18) -0.00380(14) -0.00286(14) -0.00187(14) P1 0.0135(3) 0.0121(3) 0.0097(3) -0.0026(3) -0.0015(3) -0.0021(3) P2 0.0122(3) 0.0122(3) 0.0116(4) -0.0046(3) -0.0018(3) -0.0011(3) P3 0.0125(3) 0.0111(3) 0.0107(4) -0.0032(3) -0.0029(3) -0.0014(3) P4 0.0125(3) 0.0116(3) 0.0098(3) -0.0025(3) -0.0015(3) -0.0020(3) N1 0.0110(11) 0.0115(11) 0.0099(11) -0.0022(9) -0.0022(9) -0.0004(9) N2 0.0195(12) 0.0122(11) 0.0098(12) -0.0025(10) -0.0031(10) -0.0017(10) N3 0.0173(12) 0.0115(11) 0.0162(13) -0.0031(10) -0.0035(10) -0.0007(10) N4 0.0268(14) 0.0185(13) 0.0149(13) -0.0072(11) -0.0064(11) -0.0002(11) N5 0.0163(12) 0.0133(12) 0.0155(13) -0.0064(10) -0.0047(10) 0.0006(10) N6 0.0184(13) 0.0179(13) 0.0370(17) -0.0167(12) -0.0041(12) 0.0025(11) N7 0.0111(11) 0.0139(11) 0.0123(12) -0.0062(10) -0.0008(9) -0.0025(9) N8 0.0099(11) 0.0136(11) 0.0115(12) -0.0048(10) -0.0016(9) -0.0017(9) N9 0.0169(12) 0.0128(11) 0.0112(12) -0.0039(10) -0.0051(10) -0.0002(10) N10 0.0195(12) 0.0163(12) 0.0102(12) -0.0011(10) -0.0039(10) -0.0025(10) N11 0.0183(13) 0.0179(13) 0.0188(14) -0.0070(11) -0.0052(11) 0.0004(10) N12 0.0096(11) 0.0134(11) 0.0119(12) -0.0030(10) -0.0010(9) -0.0015(9) N13 0.0152(11) 0.0121(11) 0.0093(12) -0.0016(9) -0.0035(9) -0.0031(10) N14 0.0178(12) 0.0203(13) 0.0138(13) -0.0052(11) -0.0082(10) -0.0018(10) C1 0.0139(13) 0.0158(14) 0.0121(14) -0.0042(12) 0.0011(11) -0.0019(11) C2 0.0199(15) 0.0219(16) 0.0140(15) -0.0009(13) 0.0017(12) -0.0042(13) C3 0.0197(15) 0.0196(15) 0.0162(15) -0.0069(13) -0.0014(12) 0.0000(13) C4 0.0140(14) 0.0227(16) 0.0181(16) -0.0042(13) 0.0000(12) -0.0016(12) C5 0.0205(15) 0.0157(14) 0.0153(15) -0.0039(12) -0.0061(12) -0.0015(12) C6 0.0230(15) 0.0146(14) 0.0146(15) -0.0057(12) -0.0026(12) -0.0018(12) C7 0.0213(15) 0.0134(14) 0.0101(14) -0.0017(11) -0.0008(12) -0.0036(12) C8 0.0200(15) 0.0154(14) 0.0146(15) -0.0024(12) -0.0042(12) -0.0024(12) C9 0.0250(16) 0.0155(15) 0.0236(17) -0.0052(13) -0.0037(13) 0.0016(13) C10 0.0206(15) 0.0207(15) 0.0175(16) -0.0106(13) -0.0060(12) 0.0035(13) C11 0.0304(18) 0.0201(16) 0.0245(18) -0.0054(14) -0.0015(14) -0.0051(14) C12 0.0195(15) 0.0177(15) 0.0216(16) -0.0101(13) -0.0067(13) -0.0015(12) C13 0.0242(16) 0.0278(17) 0.0271(18) -0.0189(15) -0.0027(14) -0.0042(14) C14 0.0209(16) 0.0169(15) 0.0329(19) -0.0114(14) -0.0097(14) 0.0027(13) C15 0.0248(16) 0.0157(14) 0.0195(16) -0.0059(13) -0.0053(13) 0.0005(13) C16 0.0290(19) 0.033(2) 0.060(3) -0.034(2) -0.0101(18) 0.0058(16) C17 0.0123(13) 0.0152(14) 0.0143(14) -0.0046(12) -0.0008(11) -0.0040(11) C18 0.0160(14) 0.0185(15) 0.0211(16) -0.0087(13) -0.0031(12) 0.0001(12) C19 0.0166(15) 0.0276(17) 0.0165(16) -0.0044(13) 0.0025(12) -0.0048(13) C20 0.0185(15) 0.0203(15) 0.0259(17) -0.0117(14) -0.0007(13) -0.0049(13) C21 0.0125(13) 0.0156(14) 0.0147(14) -0.0041(12) -0.0005(11) -0.0031(11) C22 0.0183(15) 0.0146(14) 0.0164(15) -0.0021(12) -0.0017(12) -0.0034(12) C23 0.0168(14) 0.0173(15) 0.0259(17) -0.0096(13) 0.0032(13) -0.0025(12) C24 0.0143(14) 0.0214(15) 0.0194(16) -0.0038(13) -0.0049(12) -0.0033(12) C25 0.0216(15) 0.0143(14) 0.0152(15) -0.0045(12) -0.0050(12) 0.0017(12) C26 0.0241(16) 0.0115(14) 0.0158(15) -0.0004(12) -0.0067(12) -0.0003(12) C27 0.0198(15) 0.0187(15) 0.0175(16) -0.0079(13) -0.0054(12) -0.0027(12) C28 0.0233(15) 0.0167(14) 0.0158(15) -0.0043(12) -0.0054(12) -0.0064(13) C29 0.0253(16) 0.0239(16) 0.0123(15) -0.0003(13) -0.0033(13) -0.0036(14) C30 0.0200(15) 0.0157(14) 0.0227(17) -0.0077(13) -0.0092(13) 0.0016(12) C31 0.043(2) 0.0268(18) 0.0168(17) -0.0056(14) -0.0087(15) -0.0028(16) C32 0.0144(14) 0.0166(14) 0.0114(14) -0.0037(12) -0.0017(11) -0.0024(12) C33 0.0181(15) 0.0227(16) 0.0237(17) -0.0081(14) 0.0004(13) -0.0049(13) C34 0.0168(15) 0.0228(16) 0.0232(17) -0.0042(14) 0.0030(13) 0.0002(13) C35 0.0166(15) 0.0320(18) 0.0116(15) -0.0037(13) 0.0003(12) -0.0042(13) C36 0.0187(14) 0.0153(14) 0.0101(14) -0.0024(12) -0.0028(11) -0.0028(12) C37 0.0206(15) 0.0165(14) 0.0156(15) -0.0046(12) -0.0046(12) -0.0003(12) C38 0.0198(15) 0.0142(14) 0.0170(15) -0.0033(12) -0.0046(12) -0.0047(12) C39 0.0204(15) 0.0134(14) 0.0141(15) -0.0032(12) -0.0075(12) -0.0004(12) C40 0.0255(17) 0.0294(18) 0.0265(18) -0.0084(15) -0.0136(14) -0.0034(14) C41 0.044(2) 0.0303(19) 0.031(2) -0.0147(17) 0.0086(17) -0.0118(17) Cl1 0.0408(5) 0.0365(5) 0.0454(6) -0.0156(4) -0.0097(4) -0.0055(4) Cl2 0.0343(5) 0.0424(5) 0.0426(6) -0.0187(5) -0.0068(4) 0.0004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu2 2.5551(4) . ? I1 Cu1 2.6865(4) . ? I2 Cu2 2.5722(4) . ? I2 Cu1 2.7246(4) . ? I3 Cu4 2.5500(4) . ? I3 Cu3 2.6975(4) . ? I4 Cu4 2.5888(4) . ? I4 Cu3 2.7240(4) . ? Cu1 N4 2.024(2) . ? Cu1 P1 2.2205(8) . ? Cu2 P2 2.2036(8) . ? Cu3 N11 2.028(3) . ? Cu3 P3 2.2357(8) . ? Cu3 Cu4 2.7974(5) . ? Cu4 P4 2.2086(8) . ? P1 N2 1.660(2) . ? P1 N12 1.703(2) 2_767 ? P1 N1 1.725(2) . ? P1 P4 2.5734(10) 2_767 ? P2 N5 1.656(2) . ? P2 N8 1.699(2) . ? P2 N7 1.717(2) . ? P2 P3 2.5656(10) . ? P3 N9 1.658(2) . ? P3 N7 1.713(2) . ? P3 N8 1.738(2) . ? P4 N13 1.663(2) . ? P4 N1 1.694(2) 2_767 ? P4 N12 1.726(2) . ? P4 P1 2.5734(10) 2_767 ? N1 C1 1.488(3) . ? N1 P4 1.694(2) 2_767 ? N2 C5 1.457(3) . ? N2 C7 1.467(3) . ? N3 C9 1.455(4) . ? N3 C6 1.467(3) . ? N3 C8 1.467(3) . ? N4 C10 1.140(4) . ? N5 C12 1.458(3) . ? N5 C15 1.473(4) . ? N6 C14 1.455(4) . ? N6 C13 1.458(4) . ? N6 C16 1.460(4) . ? N7 C17 1.497(3) . ? N8 C21 1.489(3) . ? N9 C25 1.462(3) . ? N9 C28 1.470(3) . ? N10 C29 1.454(3) . ? N10 C26 1.465(3) . ? N10 C27 1.467(3) . ? N11 C30 1.125(4) . ? N12 C32 1.484(3) . ? N12 P1 1.704(2) 2_767 ? N13 C39 1.466(3) . ? N13 C36 1.470(3) . ? N14 C37 1.461(3) . ? N14 C38 1.465(3) . ? N14 C40 1.468(3) . ? C1 C2 1.527(4) . ? C1 C4 1.532(4) . ? C1 C3 1.535(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.521(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.511(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.459(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.514(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.516(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.524(4) . ? C17 C18 1.527(4) . ? C17 C20 1.528(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.528(4) . ? C21 C22 1.530(4) . ? C21 C24 1.534(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.521(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.512(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.468(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.522(4) . ? C32 C35 1.527(4) . ? C32 C33 1.538(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.515(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.515(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 Cl1 1.748(3) . ? C41 Cl2 1.801(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu2 I1 Cu1 80.478(13) . . ? Cu2 I2 Cu1 79.455(13) . . ? Cu4 I3 Cu3 64.358(12) . . ? Cu4 I4 Cu3 63.484(12) . . ? N4 Cu1 P1 113.34(7) . . ? N4 Cu1 I1 102.98(7) . . ? P1 Cu1 I1 114.08(2) . . ? N4 Cu1 I2 107.45(7) . . ? P1 Cu1 I2 120.19(2) . . ? I1 Cu1 I2 96.353(13) . . ? P2 Cu2 I1 124.55(2) . . ? P2 Cu2 I2 131.49(2) . . ? I1 Cu2 I2 103.713(14) . . ? N11 Cu3 P3 110.64(7) . . ? N11 Cu3 I3 109.70(7) . . ? P3 Cu3 I3 117.34(2) . . ? N11 Cu3 I4 102.19(7) . . ? P3 Cu3 I4 115.42(2) . . ? I3 Cu3 I4 100.138(13) . . ? N11 Cu3 Cu4 87.13(7) . . ? P3 Cu3 Cu4 162.08(3) . . ? I3 Cu3 Cu4 55.263(10) . . ? I4 Cu3 Cu4 55.901(11) . . ? P4 Cu4 I3 132.80(2) . . ? P4 Cu4 I4 118.10(2) . . ? I3 Cu4 I4 108.000(15) . . ? P4 Cu4 Cu3 155.17(3) . . ? I3 Cu4 Cu3 60.380(12) . . ? I4 Cu4 Cu3 60.615(11) . . ? N2 P1 N12 106.67(11) . 2_767 ? N2 P1 N1 111.58(11) . . ? N12 P1 N1 81.11(11) 2_767 . ? N2 P1 Cu1 113.48(9) . . ? N12 P1 Cu1 120.57(8) 2_767 . ? N1 P1 Cu1 119.16(8) . . ? N2 P1 P4 123.65(9) . 2_767 ? N12 P1 P4 41.72(8) 2_767 2_767 ? N1 P1 P4 40.72(8) . 2_767 ? Cu1 P1 P4 122.82(4) . 2_767 ? N5 P2 N8 109.99(12) . . ? N5 P2 N7 110.50(12) . . ? N8 P2 N7 81.27(11) . . ? N5 P2 Cu2 108.92(9) . . ? N8 P2 Cu2 121.64(8) . . ? N7 P2 Cu2 121.92(8) . . ? N5 P2 P3 128.38(9) . . ? N8 P2 P3 42.29(8) . . ? N7 P2 P3 41.52(7) . . ? Cu2 P2 P3 122.70(4) . . ? N9 P3 N7 107.91(11) . . ? N9 P3 N8 112.98(12) . . ? N7 P3 N8 80.28(10) . . ? N9 P3 Cu3 112.24(8) . . ? N7 P3 Cu3 121.58(8) . . ? N8 P3 Cu3 118.10(8) . . ? N9 P3 P2 128.20(9) . . ? N7 P3 P2 41.63(8) . . ? N8 P3 P2 41.14(7) . . ? Cu3 P3 P2 119.54(3) . . ? N13 P4 N1 107.17(11) . 2_767 ? N13 P4 N12 112.14(11) . . ? N1 P4 N12 81.35(11) 2_767 . ? N13 P4 Cu4 105.85(8) . . ? N1 P4 Cu4 122.64(8) 2_767 . ? N12 P4 Cu4 125.51(8) . . ? N13 P4 P1 124.45(8) . 2_767 ? N1 P4 P1 41.64(8) 2_767 2_767 ? N12 P4 P1 41.05(8) . 2_767 ? Cu4 P4 P1 129.47(4) . 2_767 ? C1 N1 P4 129.59(18) . 2_767 ? C1 N1 P1 126.61(18) . . ? P4 N1 P1 97.64(11) 2_767 . ? C5 N2 C7 111.8(2) . . ? C5 N2 P1 125.42(19) . . ? C7 N2 P1 120.05(18) . . ? C9 N3 C6 109.0(2) . . ? C9 N3 C8 110.8(2) . . ? C6 N3 C8 109.1(2) . . ? C10 N4 Cu1 161.1(2) . . ? C12 N5 C15 112.2(2) . . ? C12 N5 P2 121.20(19) . . ? C15 N5 P2 124.13(19) . . ? C14 N6 C13 109.5(2) . . ? C14 N6 C16 110.1(2) . . ? C13 N6 C16 110.4(3) . . ? C17 N7 P3 129.49(18) . . ? C17 N7 P2 127.04(18) . . ? P3 N7 P2 96.86(11) . . ? C21 N8 P2 128.51(18) . . ? C21 N8 P3 127.98(18) . . ? P2 N8 P3 96.57(11) . . ? C25 N9 C28 112.5(2) . . ? C25 N9 P3 126.15(19) . . ? C28 N9 P3 118.83(18) . . ? C29 N10 C26 110.8(2) . . ? C29 N10 C27 109.9(2) . . ? C26 N10 C27 108.9(2) . . ? C30 N11 Cu3 159.7(2) . . ? C32 N12 P1 130.68(18) . 2_767 ? C32 N12 P4 127.87(18) . . ? P1 N12 P4 97.23(11) 2_767 . ? C39 N13 C36 112.8(2) . . ? C39 N13 P4 124.17(18) . . ? C36 N13 P4 119.74(17) . . ? C37 N14 C38 109.4(2) . . ? C37 N14 C40 110.2(2) . . ? C38 N14 C40 111.5(2) . . ? N1 C1 C2 107.1(2) . . ? N1 C1 C4 108.9(2) . . ? C2 C1 C4 110.0(2) . . ? N1 C1 C3 110.9(2) . . ? C2 C1 C3 110.2(2) . . ? C4 C1 C3 109.7(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 110.0(2) . . ? N2 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? N2 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N3 C6 C5 111.6(2) . . ? N3 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N3 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 110.2(2) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C7 110.7(2) . . ? N3 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C11 178.2(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 110.3(2) . . ? N5 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? N5 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N6 C13 C12 110.3(3) . . ? N6 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? N6 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N6 C14 C15 111.9(2) . . ? N6 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? N6 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? N5 C15 C14 110.0(2) . . ? N5 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N5 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N7 C17 C19 108.0(2) . . ? N7 C17 C18 111.1(2) . . ? C19 C17 C18 110.9(2) . . ? N7 C17 C20 108.0(2) . . ? C19 C17 C20 109.3(2) . . ? C18 C17 C20 109.5(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N8 C21 C23 108.3(2) . . ? N8 C21 C22 112.3(2) . . ? C23 C21 C22 109.7(2) . . ? N8 C21 C24 107.9(2) . . ? C23 C21 C24 109.2(2) . . ? C22 C21 C24 109.4(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N9 C25 C26 110.1(2) . . ? N9 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N9 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N10 C26 C25 111.8(2) . . ? N10 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? N10 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 107.9 . . ? N10 C27 C28 110.4(2) . . ? N10 C27 H27A 109.6 . . ? C28 C27 H27A 109.6 . . ? N10 C27 H27B 109.6 . . ? C28 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? N9 C28 C27 110.5(2) . . ? N9 C28 H28A 109.5 . . ? C27 C28 H28A 109.5 . . ? N9 C28 H28B 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? N10 C29 H29A 109.5 . . ? N10 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N10 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N11 C30 C31 178.2(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N12 C32 C34 109.0(2) . . ? N12 C32 C35 107.5(2) . . ? C34 C32 C35 109.7(2) . . ? N12 C32 C33 111.6(2) . . ? C34 C32 C33 109.5(2) . . ? C35 C32 C33 109.6(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N13 C36 C37 110.4(2) . . ? N13 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? N13 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? N14 C37 C36 110.3(2) . . ? N14 C37 H37A 109.6 . . ? C36 C37 H37A 109.6 . . ? N14 C37 H37B 109.6 . . ? C36 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? N14 C38 C39 109.7(2) . . ? N14 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? N14 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? N13 C39 C38 109.9(2) . . ? N13 C39 H39A 109.7 . . ? C38 C39 H39A 109.7 . . ? N13 C39 H39B 109.7 . . ? C38 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? N14 C40 H40A 109.5 . . ? N14 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N14 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Cl1 C41 Cl2 110.49(19) . . ? Cl1 C41 H41A 109.6 . . ? Cl2 C41 H41A 109.6 . . ? Cl1 C41 H41B 109.6 . . ? Cl2 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.235 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.182 # Attachment 'Compound_12.cif' data_msb350a_0m _database_code_depnum_ccdc_archive 'CCDC 678206' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H90 Cu4 I4 N14 O4 P4' _chemical_formula_sum 'C56 H90 Cu4 I4 N14 O4 P4' _chemical_formula_weight 1909.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 22.928(1) _cell_length_b 14.8182(7) _cell_length_c 21.085(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7163.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9630 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.42 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3776 _exptl_absorpt_coefficient_mu 3.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7175 _exptl_absorpt_correction_T_max 0.8459 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames (0.3 deg. width in omega) at phi = 0, 120 and 240 deg. A scan time of 60 sec/frame was used. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61113 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.72 _reflns_number_total 8837 _reflns_number_gt 7505 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/2. University of G\"ottingen, Germany. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+12.5283P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8837 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0623 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 I1 I 0.7500 0.2500 0.214488(11) 0.01114(5) Uani 1 2 d S . . Cu1 Cu 0.650336(13) 0.26488(2) 0.135485(14) 0.01076(7) Uani 1 1 d . . . P1 P 0.69431(3) 0.25860(4) 0.04326(3) 0.00962(12) Uani 1 1 d . . . O1 O 0.57420(9) 0.32350(16) -0.11815(10) 0.0263(5) Uani 1 1 d . . . N1 N 0.74574(9) 0.17529(14) 0.03151(10) 0.0105(4) Uani 1 1 d . . . N2 N 0.65056(9) 0.26807(15) -0.01903(10) 0.0144(5) Uani 1 1 d . . . N3 N 0.59330(9) 0.16883(15) 0.17183(10) 0.0128(4) Uani 1 1 d . . . N4 N 0.60479(9) 0.36960(14) 0.17716(10) 0.0125(4) Uani 1 1 d . . . C1 C 0.73873(11) 0.07547(17) 0.03449(12) 0.0128(5) Uani 1 1 d . . . C2 C 0.72040(14) 0.04244(19) -0.03114(13) 0.0225(6) Uani 1 1 d . . . H2A H 0.6828 0.0694 -0.0425 0.034 Uiso 1 1 calc R . . H2B H 0.7167 -0.0234 -0.0306 0.034 Uiso 1 1 calc R . . H2C H 0.7499 0.0601 -0.0624 0.034 Uiso 1 1 calc R . . C3 C 0.79685(12) 0.03179(18) 0.05220(14) 0.0194(6) Uani 1 1 d . . . H3A H 0.8264 0.0479 0.0206 0.029 Uiso 1 1 calc R . . H3B H 0.7923 -0.0339 0.0534 0.029 Uiso 1 1 calc R . . H3C H 0.8092 0.0534 0.0940 0.029 Uiso 1 1 calc R . . C4 C 0.69235(12) 0.04969(18) 0.08296(13) 0.0189(6) Uani 1 1 d . . . H4A H 0.7034 0.0731 0.1247 0.028 Uiso 1 1 calc R . . H4B H 0.6890 -0.0162 0.0850 0.028 Uiso 1 1 calc R . . H4C H 0.6548 0.0755 0.0703 0.028 Uiso 1 1 calc R . . C5 C 0.66965(13) 0.2698(2) -0.08519(12) 0.0219(6) Uani 1 1 d . . . H5A H 0.6641 0.2094 -0.1043 0.026 Uiso 1 1 calc R . . H5B H 0.7117 0.2847 -0.0871 0.026 Uiso 1 1 calc R . . C6 C 0.63541(12) 0.3388(2) -0.12217(14) 0.0256(7) Uani 1 1 d . . . H6A H 0.6444 0.3998 -0.1057 0.031 Uiso 1 1 calc R . . H6B H 0.6475 0.3367 -0.1672 0.031 Uiso 1 1 calc R . . C7 C 0.55611(12) 0.3289(2) -0.05318(14) 0.0231(6) Uani 1 1 d . . . H7A H 0.5134 0.3194 -0.0505 0.028 Uiso 1 1 calc R . . H7B H 0.5649 0.3898 -0.0364 0.028 Uiso 1 1 calc R . . C8 C 0.58697(11) 0.2586(2) -0.01336(13) 0.0173(6) Uani 1 1 d . . . H8A H 0.5754 0.2657 0.0316 0.021 Uiso 1 1 calc R . . H8B H 0.5751 0.1976 -0.0275 0.021 Uiso 1 1 calc R . . C9 C 0.60925(11) 0.11236(17) 0.21871(12) 0.0127(5) Uani 1 1 d . . . H9 H 0.6490 0.1115 0.2313 0.015 Uiso 1 1 calc R . . C10 C 0.57064(11) 0.05547(17) 0.24957(12) 0.0129(5) Uani 1 1 d . . . H10 H 0.5836 0.0188 0.2837 0.015 Uiso 1 1 calc R . . C11 C 0.51257(11) 0.05249(17) 0.23020(12) 0.0133(5) Uani 1 1 d . . . C12 C 0.49624(12) 0.10882(19) 0.18081(13) 0.0178(6) Uani 1 1 d . . . H12 H 0.4573 0.1077 0.1654 0.021 Uiso 1 1 calc R . . C13 C 0.53680(12) 0.16694(19) 0.15396(13) 0.0168(5) Uani 1 1 d . . . H13 H 0.5242 0.2071 0.1216 0.020 Uiso 1 1 calc R . . C14 C 0.60045(11) 0.37257(18) 0.24087(12) 0.0143(5) Uani 1 1 d . . . H14 H 0.6236 0.3321 0.2651 0.017 Uiso 1 1 calc R . . C15 C 0.56413(11) 0.43144(18) 0.27279(13) 0.0145(5) Uani 1 1 d . . . H15 H 0.5630 0.4317 0.3178 0.017 Uiso 1 1 calc R . . C16 C 0.52903(11) 0.49064(18) 0.23815(12) 0.0128(5) Uani 1 1 d . . . C17 C 0.53314(11) 0.48808(18) 0.17233(13) 0.0145(5) Uani 1 1 d . . . H17 H 0.5100 0.5271 0.1470 0.017 Uiso 1 1 calc R . . C18 C 0.57150(11) 0.42781(18) 0.14412(13) 0.0145(5) Uani 1 1 d . . . H18 H 0.5744 0.4276 0.0992 0.017 Uiso 1 1 calc R . . I2 I 0.7500 0.7500 0.456611(12) 0.01698(6) Uani 1 2 d S . . I3 I 0.574553(8) 0.859385(15) 0.429589(9) 0.02619(6) Uani 1 1 d . . . Cu2 Cu 0.661904(15) 0.78866(2) 0.379947(16) 0.01640(7) Uani 1 1 d . . . P2 P 0.69514(3) 0.76410(4) 0.28287(3) 0.01174(13) Uani 1 1 d . . . O2 O 0.56837(9) 0.75411(15) 0.12068(10) 0.0248(5) Uani 1 1 d . . . N5 N 0.74138(9) 0.67575(14) 0.27105(10) 0.0123(4) Uani 1 1 d . . . N6 N 0.65064(10) 0.76795(15) 0.22069(11) 0.0150(5) Uani 1 1 d . . . C19 C 0.72981(12) 0.57810(17) 0.28032(13) 0.0141(5) Uani 1 1 d . . . C20 C 0.78435(13) 0.5316(2) 0.30526(17) 0.0260(7) Uani 1 1 d . . . H20A H 0.7944 0.5565 0.3469 0.039 Uiso 1 1 calc R . . H20B H 0.8167 0.5417 0.2757 0.039 Uiso 1 1 calc R . . H20C H 0.7771 0.4667 0.3092 0.039 Uiso 1 1 calc R . . C21 C 0.71391(15) 0.5378(2) 0.21599(14) 0.0248(7) Uani 1 1 d . . . H21A H 0.7101 0.4722 0.2200 0.037 Uiso 1 1 calc R . . H21B H 0.7446 0.5520 0.1852 0.037 Uiso 1 1 calc R . . H21C H 0.6768 0.5634 0.2015 0.037 Uiso 1 1 calc R . . C22 C 0.68004(12) 0.56395(19) 0.32690(13) 0.0185(6) Uani 1 1 d . . . H22A H 0.6902 0.5913 0.3678 0.028 Uiso 1 1 calc R . . H22B H 0.6733 0.4992 0.3327 0.028 Uiso 1 1 calc R . . H22C H 0.6446 0.5923 0.3103 0.028 Uiso 1 1 calc R . . C23 C 0.59256(12) 0.80916(19) 0.22571(14) 0.0180(6) Uani 1 1 d . . . H23A H 0.5941 0.8726 0.2111 0.022 Uiso 1 1 calc R . . H23B H 0.5795 0.8086 0.2704 0.022 Uiso 1 1 calc R . . C24 C 0.55000(13) 0.7558(2) 0.18481(14) 0.0233(6) Uani 1 1 d . . . H24A H 0.5472 0.6932 0.2010 0.028 Uiso 1 1 calc R . . H24B H 0.5108 0.7836 0.1875 0.028 Uiso 1 1 calc R . . C25 C 0.62341(12) 0.7092(2) 0.11581(14) 0.0215(6) Uani 1 1 d . . . H25A H 0.6355 0.7069 0.0708 0.026 Uiso 1 1 calc R . . H25B H 0.6194 0.6465 0.1313 0.026 Uiso 1 1 calc R . . C26 C 0.67004(12) 0.7577(2) 0.15432(12) 0.0184(6) Uani 1 1 d . . . H26A H 0.7068 0.7227 0.1530 0.022 Uiso 1 1 calc R . . H26B H 0.6776 0.8179 0.1357 0.022 Uiso 1 1 calc R . . N7 N 0.55923(17) 0.4734(2) 0.43591(16) 0.0497(9) Uani 1 1 d . . . C27 C 0.56675(18) 0.5342(3) 0.46868(18) 0.0414(9) Uani 1 1 d . . . C28 C 0.5744(2) 0.6098(3) 0.5111(2) 0.0546(12) Uani 1 1 d . . . H28A H 0.5536 0.5981 0.5508 0.082 Uiso 1 1 calc R . . H28B H 0.5588 0.6645 0.4912 0.082 Uiso 1 1 calc R . . H28C H 0.6160 0.6180 0.5199 0.082 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.00863(10) 0.01307(11) 0.01172(11) 0.000 0.000 -0.00048(8) Cu1 0.01064(14) 0.01055(15) 0.01109(15) -0.00020(11) 0.00255(11) -0.00020(11) P1 0.0090(3) 0.0107(3) 0.0091(3) 0.0005(2) -0.0006(2) -0.0003(2) O1 0.0142(10) 0.0466(14) 0.0182(10) 0.0100(10) -0.0058(8) -0.0032(9) N1 0.0100(10) 0.0104(10) 0.0110(10) -0.0006(8) -0.0001(8) -0.0007(8) N2 0.0105(10) 0.0224(12) 0.0102(10) 0.0014(9) 0.0004(8) 0.0005(9) N3 0.0124(10) 0.0129(11) 0.0130(11) -0.0008(8) 0.0017(8) -0.0021(8) N4 0.0096(10) 0.0122(10) 0.0159(11) -0.0013(8) 0.0011(8) -0.0014(8) C1 0.0154(13) 0.0088(12) 0.0141(12) -0.0032(9) -0.0005(10) -0.0016(10) C2 0.0326(17) 0.0168(14) 0.0179(14) -0.0078(11) -0.0034(12) -0.0021(12) C3 0.0170(14) 0.0137(13) 0.0276(15) -0.0004(11) -0.0012(11) 0.0022(11) C4 0.0211(14) 0.0128(13) 0.0228(15) 0.0010(11) 0.0041(11) -0.0016(11) C5 0.0205(14) 0.0368(18) 0.0082(12) 0.0009(11) -0.0006(11) 0.0038(13) C6 0.0165(14) 0.0422(19) 0.0180(15) 0.0116(13) -0.0032(11) -0.0026(13) C7 0.0128(13) 0.0366(17) 0.0200(15) 0.0091(13) -0.0019(11) 0.0018(12) C8 0.0126(12) 0.0234(14) 0.0159(13) 0.0030(11) -0.0033(10) -0.0043(11) C9 0.0115(12) 0.0135(12) 0.0133(12) 0.0005(10) 0.0004(10) -0.0014(10) C10 0.0134(12) 0.0142(12) 0.0111(12) 0.0008(10) 0.0002(10) 0.0014(10) C11 0.0128(12) 0.0128(12) 0.0143(12) -0.0017(10) 0.0028(10) -0.0024(10) C12 0.0101(12) 0.0246(15) 0.0187(14) 0.0047(11) -0.0011(10) -0.0022(11) C13 0.0128(12) 0.0195(14) 0.0180(14) 0.0054(11) -0.0012(10) -0.0006(10) C14 0.0128(12) 0.0149(13) 0.0152(13) 0.0006(10) 0.0001(10) 0.0016(10) C15 0.0114(12) 0.0187(13) 0.0135(13) -0.0027(10) 0.0005(10) 0.0000(10) C16 0.0085(12) 0.0140(12) 0.0159(13) -0.0025(10) -0.0002(10) -0.0017(10) C17 0.0122(12) 0.0136(13) 0.0176(13) 0.0007(10) -0.0017(10) 0.0020(10) C18 0.0134(12) 0.0151(13) 0.0150(13) -0.0016(10) 0.0018(10) 0.0005(10) I2 0.01521(12) 0.02092(13) 0.01481(12) 0.000 0.000 0.00222(10) I3 0.01759(9) 0.03829(12) 0.02270(10) -0.00250(8) 0.00266(8) 0.01034(8) Cu2 0.01485(16) 0.01835(17) 0.01600(16) -0.00122(13) 0.00265(13) 0.00149(13) P2 0.0108(3) 0.0113(3) 0.0131(3) -0.0004(2) -0.0008(2) 0.0008(2) O2 0.0195(10) 0.0343(12) 0.0206(10) -0.0024(9) -0.0066(8) 0.0018(9) N5 0.0108(10) 0.0105(10) 0.0156(11) -0.0015(8) 0.0018(8) 0.0013(8) N6 0.0131(11) 0.0167(11) 0.0152(11) -0.0007(9) -0.0031(9) 0.0004(9) C19 0.0147(12) 0.0101(12) 0.0174(13) 0.0002(10) 0.0017(10) 0.0005(10) C20 0.0179(15) 0.0154(14) 0.0448(19) 0.0040(13) -0.0020(13) 0.0035(12) C21 0.0406(18) 0.0146(14) 0.0191(15) -0.0020(11) 0.0027(13) -0.0062(13) C22 0.0205(14) 0.0163(13) 0.0187(14) 0.0004(11) 0.0032(11) -0.0031(11) C23 0.0140(13) 0.0179(14) 0.0223(15) -0.0037(11) -0.0041(11) 0.0037(11) C24 0.0148(13) 0.0314(16) 0.0236(15) -0.0031(13) -0.0039(11) 0.0006(12) C25 0.0190(14) 0.0296(16) 0.0158(14) -0.0031(12) -0.0019(11) 0.0012(12) C26 0.0165(13) 0.0258(15) 0.0130(13) 0.0012(11) -0.0020(10) -0.0016(11) N7 0.064(2) 0.048(2) 0.0361(18) -0.0029(16) 0.0002(17) 0.0111(18) C27 0.053(2) 0.037(2) 0.034(2) -0.0004(17) -0.0034(17) 0.0159(18) C28 0.061(3) 0.031(2) 0.071(3) -0.012(2) -0.022(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.8364(3) . ? I1 Cu1 2.8364(4) 2_655 ? Cu1 N4 2.067(2) . ? Cu1 N3 2.079(2) . ? Cu1 P1 2.1924(7) . ? P1 N2 1.659(2) . ? P1 N1 1.706(2) 2_655 ? P1 N1 1.725(2) . ? P1 P1 2.5663(13) 2_655 ? O1 C6 1.424(3) . ? O1 C7 1.434(4) . ? N1 C1 1.489(3) . ? N1 P1 1.706(2) 2_655 ? N2 C5 1.462(3) . ? N2 C8 1.470(3) . ? N3 C9 1.346(3) . ? N3 C13 1.349(3) . ? N4 C18 1.346(3) . ? N4 C14 1.348(3) . ? C1 C4 1.523(4) . ? C1 C2 1.527(4) . ? C1 C3 1.528(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.507(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.513(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.393(4) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 C16 1.482(4) 3_645 ? C12 C13 1.388(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.397(4) . ? C15 H15 0.9500 . ? C16 C17 1.391(4) . ? C16 C11 1.482(4) 3_655 ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? I2 Cu2 2.6497(4) . ? I2 Cu2 2.6498(4) 2_665 ? I3 Cu2 2.4910(4) . ? Cu2 P2 2.2143(7) . ? P2 N6 1.662(2) . ? P2 N5 1.703(2) . ? P2 N5 1.725(2) 2_665 ? P2 P2 2.5502(13) 2_665 ? O2 C24 1.417(4) . ? O2 C25 1.430(3) . ? N5 C19 1.484(3) . ? N5 P2 1.725(2) 2_665 ? N6 C23 1.469(3) . ? N6 C26 1.476(3) . ? C19 C22 1.520(4) . ? C19 C20 1.521(4) . ? C19 C21 1.526(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.524(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.522(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N7 C27 1.148(5) . ? C27 C28 1.443(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu1 I1 Cu1 108.069(15) . 2_655 ? N4 Cu1 N3 92.26(9) . . ? N4 Cu1 P1 129.90(6) . . ? N3 Cu1 P1 125.95(6) . . ? N4 Cu1 I1 102.46(6) . . ? N3 Cu1 I1 103.71(6) . . ? P1 Cu1 I1 98.46(2) . . ? N2 P1 N1 108.88(11) . 2_655 ? N2 P1 N1 111.11(11) . . ? N1 P1 N1 80.76(11) 2_655 . ? N2 P1 Cu1 114.87(8) . . ? N1 P1 Cu1 118.36(8) 2_655 . ? N1 P1 Cu1 118.17(8) . . ? N2 P1 P1 127.60(8) . 2_655 ? N1 P1 P1 41.87(7) 2_655 2_655 ? N1 P1 P1 41.30(7) . 2_655 ? Cu1 P1 P1 117.506(18) . 2_655 ? C6 O1 C7 109.5(2) . . ? C1 N1 P1 130.63(17) . 2_655 ? C1 N1 P1 129.12(17) . . ? P1 N1 P1 96.83(11) 2_655 . ? C5 N2 C8 112.1(2) . . ? C5 N2 P1 125.16(18) . . ? C8 N2 P1 121.84(18) . . ? C9 N3 C13 116.9(2) . . ? C9 N3 Cu1 121.69(17) . . ? C13 N3 Cu1 121.01(18) . . ? C18 N4 C14 117.0(2) . . ? C18 N4 Cu1 123.20(18) . . ? C14 N4 Cu1 119.05(17) . . ? N1 C1 C4 110.7(2) . . ? N1 C1 C2 108.1(2) . . ? C4 C1 C2 109.6(2) . . ? N1 C1 C3 109.7(2) . . ? C4 C1 C3 109.8(2) . . ? C2 C1 C3 109.0(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C6 110.5(2) . . ? N2 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N2 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O1 C6 C5 112.0(2) . . ? O1 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? O1 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? O1 C7 C8 110.9(2) . . ? O1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? N2 C8 C7 110.7(2) . . ? N2 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N3 C9 C10 123.4(2) . . ? N3 C9 H9 118.3 . . ? C10 C9 H9 118.3 . . ? C9 C10 C11 119.5(2) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 117.3(2) . . ? C12 C11 C16 122.5(2) . 3_645 ? C10 C11 C16 120.2(2) . 3_645 ? C11 C12 C13 119.9(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? N3 C13 C12 122.8(2) . . ? N3 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? N4 C14 C15 123.4(2) . . ? N4 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C14 C15 C16 119.3(2) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 117.7(2) . . ? C17 C16 C11 120.6(2) . 3_655 ? C15 C16 C11 121.6(2) . 3_655 ? C18 C17 C16 119.2(2) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N4 C18 C17 123.4(2) . . ? N4 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? Cu2 I2 Cu2 104.812(17) . 2_665 ? P2 Cu2 I3 137.25(2) . . ? P2 Cu2 I2 105.43(2) . . ? I3 Cu2 I2 116.584(15) . . ? N6 P2 N5 107.04(11) . . ? N6 P2 N5 112.72(11) . 2_665 ? N5 P2 N5 81.42(11) . 2_665 ? N6 P2 Cu2 120.82(9) . . ? N5 P2 Cu2 118.41(8) . . ? N5 P2 Cu2 109.82(8) 2_665 . ? N6 P2 P2 127.67(8) . 2_665 ? N5 P2 P2 42.26(7) . 2_665 ? N5 P2 P2 41.60(7) 2_665 2_665 ? Cu2 P2 P2 111.50(2) . 2_665 ? C24 O2 C25 109.8(2) . . ? C19 N5 P2 128.25(17) . . ? C19 N5 P2 129.47(18) . 2_665 ? P2 N5 P2 96.14(11) . 2_665 ? C23 N6 C26 112.6(2) . . ? C23 N6 P2 120.92(18) . . ? C26 N6 P2 124.01(18) . . ? N5 C19 C22 110.7(2) . . ? N5 C19 C20 109.9(2) . . ? C22 C19 C20 109.3(2) . . ? N5 C19 C21 107.9(2) . . ? C22 C19 C21 109.9(2) . . ? C20 C19 C21 109.1(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N6 C23 C24 108.9(2) . . ? N6 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? N6 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O2 C24 C23 111.0(2) . . ? O2 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? O2 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? O2 C25 C26 111.2(2) . . ? O2 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? O2 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N6 C26 C25 110.0(2) . . ? N6 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? N6 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N7 C27 C28 178.0(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.678 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.111