# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1311 data_br611 _audit_creation_date 98-10-05 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common 'compound 3' _chemical_formula_analytical C37_H12_Cl2_Co4_O18_W2 _chemical_formula_moiety ? _chemical_formula_structural C36_H10_Co4_O18_W2_CH2Cl2 _chemical_formula_sum C37_H12_Cl2_Co4_O18_W2 _chemical_formula_weight 1418.82 _chemical_melting_point ? _computing_data_collection 'Bruker-SMART software' _computing_cell_refinement 'Bruker-SMART software' _computing_data_reduction 'Bruker-SAINT software' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 9.7530(10) _cell_length_b 11.4980(10) _cell_length_c 12.0460(15) _cell_angle_alpha 108.760(2) _cell_angle_beta 103.562(2) _cell_angle_gamma 111.034(2) _cell_volume 1096.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_measurement_reflns_used 5754 _cell_measurement_theta_min 0 _cell_measurement_theta_max 29 _cell_special_details ; ? ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _exptl_crystal_description plate _exptl_crystal_preparation ? _exptl_crystal_colour dark _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 2.149 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 668 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_coefficient_mu 6.90 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.77 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device 'Bruker CCD difractometer' _diffrn_measurement_method 'omega scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 12368 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.14 _diffrn_reflns_reduction_process ? loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 37 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 12 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 2 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Co ? 0 4 .299 .973 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 18 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 W ? 0 2 -1.421 6.872 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom W1 .873094(18) 1.137358(15) .313106(16) .04412(8) Uani ? ? Co2 .30326(6) .54881(5) .08320(5) .0424(2) Uani ? ? Co3 .49989(6) .50292(5) .20957(5) .04138(19) Uani ? ? C11 .8980(6) 1.1157(4) .4735(5) .0592(18) Uani ? ? O11 .9176(5) 1.1025(4) .5645(4) .091(2) Uani ? ? C12 .6495(6) 1.0872(5) .2124(6) .069(2) Uani ? ? O12 .5235(5) 1.0608(5) .1536(5) .113(2) Uani ? ? C13 .8476(5) 1.2964(4) .4199(5) .0572(18) Uani ? ? O13 .8282(5) 1.3845(4) .4779(4) .0836(18) Uani ? ? C21 .1400(5) .3749(5) -.0295(5) .0611(19) Uani ? ? O21 .0398(4) .2691(4) -.0992(4) .1014(19) Uani ? ? C22 .2265(6) .6043(5) .2022(5) .062(2) Uani ? ? O22 .1748(5) .6356(5) .2748(4) .103(2) Uani ? ? C23 .2793(5) .6553(5) .0072(5) .0604(19) Uani ? ? O23 .2705(6) .7258(5) -.0373(5) .108(2) Uani ? ? C31 .3826(5) .3141(5) .1416(5) .0539(17) Uani ? ? O31 .3066(5) .1973(4) .0961(4) .0896(19) Uani ? ? C32 .4852(5) .5708(5) .3627(5) .0569(18) Uani ? ? O32 .4760(5) .6136(5) .4577(4) .088(2) Uani ? ? C33 .7017(5) .5293(5) .2656(4) .0580(18) Uani ? ? O33 .8292(4) .5486(5) .3002(4) .090(2) Uani ? ? C1 .7331(4) .9203(4) .2507(4) .0450(14) Uani ? ? C2 .6478(4) .7964(4) .2105(4) .0421(13) Uani ? ? C3 .5416(4) .6543(4) .1571(4) .0389(13) Uani ? ? C4 .4866(4) .5309(3) .0552(3) .0360(12) Uani ? ? C01 1.0127(7) 1.0649(5) .1952(7) .083(3) Uani ? ? C02 .9513(7) 1.1363(6) .1427(5) .077(2) Uani ? ? C03 1.0231(6) 1.2745(5) .2386(5) .066(2) Uani ? ? C04 1.1293(6) 1.2877(5) .3496(6) .068(2) Uani ? ? C05 1.1227(6) 1.1561(6) .3233(7) .080(3) Uani ? ? Cl1 .5158(9) .9166(8) .5340(11) .188(5) Uani ? ? Cl2 .3888(11) .9944(10) .3522(10) .206(6) Uani ? ? C0 .493(3) .970(3) .428(2) .142(12) Uani ? ? H01 .98666 .96827 .15081 .10200 Uiso ? ? H02 .87097 1.09756 .05720 .09700 Uiso ? ? H03 1.00352 1.34874 .22984 .08200 Uiso ? ? H04 1.19527 1.37115 .42981 .08400 Uiso ? ? H05 1.18305 1.13267 .38058 .09900 Uiso ? ? H0a .50981 .89379 .36878 .20600 Uiso ? ? H0b .59700 1.04905 .46867 .20600 Uiso ? ? 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 W1 .04419(10) .03221(9) .05095(12) .01379(7) .01661(8) .01931(7) Co2 .0358(2) .0415(3) .0496(3) .0167(2) .0153(2) .0228(2) Co3 .0387(3) .0414(3) .0441(3) .0155(2) .0146(2) .0244(2) C11 .063(3) .043(2) .060(3) .019(2) .018(2) .022(2) O11 .118(3) .092(3) .068(3) .048(3) .031(2) .049(2) C12 .059(3) .057(3) .081(4) .023(2) .016(3) .033(3) O12 .072(3) .128(4) .125(4) .051(3) .006(3) .060(3) C13 .064(3) .043(2) .067(3) .022(2) .030(2) .028(2) O13 .111(3) .058(2) .102(3) .049(2) .062(3) .033(2) C21 .042(2) .057(3) .075(3) .021(2) .013(2) .029(3) O21 .062(2) .051(2) .121(4) .0062(17) -.010(2) .015(2) C22 .058(3) .077(3) .070(3) .040(3) .030(3) .042(3) O22 .120(4) .150(4) .099(3) .090(3) .079(3) .068(3) C23 .056(3) .064(3) .064(3) .031(2) .016(2) .033(3) O23 .121(3) .102(3) .123(4) .057(3) .029(3) .084(3) C31 .051(2) .051(2) .065(3) .023(2) .022(2) .034(2) O31 .089(3) .047(2) .120(3) .0204(18) .039(2) .038(2) C32 .056(3) .066(3) .053(3) .029(2) .019(2) .033(2) O32 .099(3) .121(3) .058(2) .060(3) .040(2) .039(2) C33 .050(2) .070(3) .052(3) .024(2) .017(2) .033(2) O33 .053(2) .131(4) .081(3) .046(2) .014(2) .048(3) C1 .042(2) .0372(19) .049(2) .0147(16) .0154(18) .0184(18) C2 .0400(18) .0394(19) .043(2) .0164(15) .0156(16) .0179(17) C3 .0356(17) .0374(18) .042(2) .0145(15) .0128(16) .0200(17) C4 .0329(16) .0327(17) .042(2) .0130(14) .0127(15) .0211(17) C01 .085(4) .047(3) .123(5) .027(3) .072(4) .029(3) C02 .081(4) .069(3) .071(4) .021(3) .043(3) .029(3) C03 .062(3) .055(3) .086(4) .020(2) .037(3) .041(3) C04 .049(2) .052(3) .093(4) .013(2) .030(3) .032(3) C05 .062(3) .083(4) .126(5) .042(3) .048(3) .065(4) Cl1 .130(5) .157(6) .221(9) .040(4) .077(5) .048(6) Cl2 .237(9) .219(9) .337(12) .161(8) .219(9) .186(10) C0 .20(2) .18(2) .112(14) .125(18) .109(16) .064(15) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 236(63) _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 4442 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .036 _refine_ls_R_factor_obs .026 _refine_ls_wR_factor_all .034 _refine_ls_wR_factor_obs .032 _refine_ls_goodness_of_fit_all .999 _refine_ls_goodness_of_fit_obs 1.039 _refine_ls_shift/esd_max .053 _refine_ls_shift/esd_mean .002 _refine_diff_density_min -1.061 _refine_diff_density_max 1.147 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C11 1.997(6) . . ? W1 C12 1.992(6) . . ? W1 C13 2.006(5) . . ? W1 C1 2.127(4) . . ? W1 C01 2.351(8) . . ? W1 C02 2.350(7) . . ? W1 C03 2.302(6) . . ? W1 C04 2.307(5) . . ? W1 C05 2.336(7) . . ? Co2 Co3 2.4794(9) . . ? Co2 C21 1.825(4) . . ? Co2 C22 1.811(6) . . ? Co2 C23 1.794(7) . . ? Co2 C3 1.995(3) . . ? Co2 C4 1.964(4) . . ? Co3 C31 1.824(4) . . ? Co3 C32 1.819(6) . . ? Co3 C33 1.800(5) . . ? Co3 C3 1.978(5) . . ? Co3 C4 1.970(5) . . ? C11 O11 1.137(8) . . ? C12 O12 1.135(7) . . ? C13 O13 1.137(7) . . ? C21 O21 1.116(5) . . ? C22 O22 1.133(9) . . ? C23 O23 1.122(9) . . ? C31 O31 1.129(5) . . ? C32 O32 1.130(7) . . ? C33 O33 1.126(7) . . ? C1 C2 1.213(5) . . ? C2 C3 1.398(5) . . ? C3 C4 1.353(5) . . ? C4 C4 1.425(6) . 2_665 ? C01 C02 1.394(11) . . ? C01 C05 1.416(8) . . ? C01 H01 .968(6) . . ? C02 C03 1.411(7) . . ? C02 H02 .974(5) . . ? C03 C04 1.411(9) . . ? C03 H03 .971(7) . . ? C04 C05 1.417(10) . . ? C04 H04 .968(4) . . ? C05 H05 .968(8) . . ? Cl1 Cl2 2.813(18) . . ? Cl1 C0 1.59(4) . . ? Cl1 H0a 1.906(13) . . ? Cl1 H0b 1.940(12) . . ? Cl1 Cl1 2.401(17) . 2_676 ? Cl1 Cl2 1.268(12) . 2_676 ? Cl1 C0 1.28(4) . 2_676 ? Cl1 H0b 1.293(10) . 2_676 ? Cl2 C0 1.37(4) . . ? Cl2 H0a 1.946(13) . . ? Cl2 H0b 1.915(10) . . ? Cl2 C0 2.46(3) . 2_676 ? C0 H0a 1.03(3) . . ? C0 H0b .95(2) . . ? C0 C0 1.60(4) . 2_676 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W1 O11 3.132(5) . . ? W1 O12 3.127(5) . . ? W1 O13 3.143(5) . . ? W1 C2 3.339(4) . . ? W1 H01 2.9909(3) . . ? W1 H02 2.9612(4) . . ? W1 H03 2.9118(3) . . ? W1 H04 2.9172(3) . . ? W1 H05 2.9656(4) . . ? Co2 O21 2.941(3) . . ? Co2 O22 2.943(6) . . ? Co2 O23 2.915(6) . . ? Co2 C31 3.293(6) . . ? Co2 C32 3.298(6) . . ? Co2 C2 3.107(3) . . ? Co2 C4 3.128(5) . 2_665 ? Co3 C21 3.407(5) . . ? Co3 C22 3.265(7) . . ? Co3 O31 2.953(3) . . ? Co3 O32 2.950(5) . . ? Co3 O33 2.926(4) . . ? Co3 C2 3.153(4) . . ? Co3 C4 3.127(4) . 2_665 ? C11 C13 2.535(9) . . ? C11 C1 2.518(5) . . ? C12 C13 2.510(5) . . ? C12 C1 2.465(9) . . ? O12 Cl2 3.157(15) . . ? C21 C22 2.832(7) . . ? C21 C23 2.845(8) . . ? C21 C4 2.922(6) . . ? O21 H01 2.496(4) . 2_665 ? C22 C23 2.713(9) . . ? C23 C3 2.770(7) . . ? C23 C4 2.921(8) . . ? C31 C32 2.895(6) . . ? C31 C33 2.820(5) . . ? C31 C4 2.945(7) . . ? C32 C33 2.752(8) . . ? O32 Cl1 3.152(11) . . ? C33 C3 2.842(8) . . ? C33 C4 2.897(7) . . ? C1 C3 2.609(5) . . ? C1 C01 2.994(9) . . ? C2 C4 2.607(4) . . ? C3 C4 2.626(5) . 2_665 ? C01 C03 2.254(9) . . ? C01 C04 2.273(7) . . ? C01 H02 2.124(8) . . ? C01 H05 2.137(7) . . ? C02 C04 2.296(7) . . ? C02 C05 2.299(10) . . ? C02 H01 2.108(8) . . ? C02 H03 2.130(6) . . ? C03 C05 2.284(11) . . ? C03 H02 2.137(4) . . ? C03 H04 2.135(5) . . ? C04 H03 2.126(7) . . ? C04 H05 2.144(7) . . ? C05 H01 2.122(5) . . ? C05 H04 2.131(6) . . ? Cl1 H0a 2.252(10) . 2_676 ? Cl2 H05 2.989(13) . 1_455 ? Cl2 H0a 2.946(11) . 2_676 ? Cl2 H0b 2.351(13) . 2_676 ? C0 H0a 2.46(3) . 2_676 ? C0 H0b 1.71(3) . 2_676 ? H0a H0b 1.55132(12) . . ? H0b H0b 2.25995(16) . 2_676 ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 W1 C12 113.0(3) . . . ? C11 W1 C13 78.6(2) . . . ? C11 W1 C1 75.19(17) . . . ? C11 W1 C01 117.2(3) . . . ? C11 W1 C02 150.8(3) . . . ? C11 W1 C03 138.47(16) . . . ? C11 W1 C04 103.8(2) . . . ? C11 W1 C05 93.2(3) . . . ? C12 W1 C13 77.8(2) . . . ? C12 W1 C1 73.4(2) . . . ? C12 W1 C01 116.1(2) . . . ? C12 W1 C02 92.9(3) . . . ? C12 W1 C03 103.5(2) . . . ? C12 W1 C04 138.1(3) . . . ? C12 W1 C05 150.5(3) . . . ? C13 W1 C1 128.8(2) . . . ? C13 W1 C01 147.4(2) . . . ? C13 W1 C02 121.9(2) . . . ? C13 W1 C03 90.9(2) . . . ? C13 W1 C04 91.0(2) . . . ? C13 W1 C05 122.56(19) . . . ? C1 W1 C01 83.76(19) . . . ? C1 W1 C02 101.11(19) . . . ? C1 W1 C03 136.34(18) . . . ? C1 W1 C04 137.5(2) . . . ? C1 W1 C05 102.2(2) . . . ? C01 W1 C02 34.5(3) . . . ? C01 W1 C03 57.9(2) . . . ? C01 W1 C04 58.43(18) . . . ? C01 W1 C05 35.2(2) . . . ? C02 W1 C03 35.30(18) . . . ? C02 W1 C04 59.07(19) . . . ? C02 W1 C05 58.8(3) . . . ? C03 W1 C04 35.7(2) . . . ? C03 W1 C05 59.0(3) . . . ? C04 W1 C05 35.5(2) . . . ? Co3 Co2 C21 103.6(2) . . . ? Co3 Co2 C22 97.9(2) . . . ? Co3 Co2 C23 144.81(15) . . . ? Co3 Co2 C3 51.10(14) . . . ? Co3 Co2 C4 51.03(13) . . . ? C21 Co2 C22 102.3(2) . . . ? C21 Co2 C23 103.6(2) . . . ? C21 Co2 C3 140.2(2) . . . ? C21 Co2 C4 100.9(2) . . . ? C22 Co2 C23 97.6(3) . . . ? C22 Co2 C3 110.49(18) . . . ? C22 Co2 C4 145.0(2) . . . ? C23 Co2 C3 93.8(2) . . . ? C23 Co2 C4 101.9(2) . . . ? C3 Co2 C4 39.98(14) . . . ? Co2 Co3 C31 98.70(17) . . . ? Co2 Co3 C32 99.1(2) . . . ? Co2 Co3 C33 147.6(2) . . . ? Co2 Co3 C3 51.68(11) . . . ? Co2 Co3 C4 50.82(13) . . . ? C31 Co3 C32 105.2(2) . . . ? C31 Co3 C33 102.2(2) . . . ? C31 Co3 C3 140.1(2) . . . ? C31 Co3 C4 101.8(2) . . . ? C32 Co3 C33 99.0(2) . . . ? C32 Co3 C3 105.5(2) . . . ? C32 Co3 C4 142.4(2) . . . ? C33 Co3 C3 97.4(2) . . . ? C33 Co3 C4 100.3(2) . . . ? C3 Co3 C4 40.09(14) . . . ? W1 C11 O11 177.1(6) . . . ? W1 C12 O12 178.2(6) . . . ? W1 C13 O13 177.9(4) . . . ? Co2 C21 O21 179.3(6) . . . ? Co2 C22 O22 178.1(4) . . . ? Co2 C23 O23 177.2(4) . . . ? Co3 C31 O31 177.6(5) . . . ? Co3 C32 O32 179.6(6) . . . ? Co3 C33 O33 178.3(6) . . . ? W1 C1 C2 176.9(4) . . . ? C1 C2 C3 175.7(5) . . . ? Co2 C3 Co3 77.22(14) . . . ? Co2 C3 C2 131.9(4) . . . ? Co2 C3 C4 68.8(2) . . . ? Co3 C3 C2 137.4(3) . . . ? Co3 C3 C4 69.6(3) . . . ? C2 C3 C4 142.7(5) . . . ? Co2 C4 Co3 78.14(17) . . . ? Co2 C4 C3 71.2(3) . . . ? Co2 C4 C4 134.2(3) . . 2_665 ? Co3 C4 C3 70.3(3) . . . ? Co3 C4 C4 133.6(3) . . 2_665 ? C3 C4 C4 141.9(4) . . 2_665 ? W1 C01 C02 72.7(4) . . . ? W1 C01 C05 71.9(4) . . . ? W1 C01 H01 123.1(6) . . . ? C02 C01 C05 109.8(5) . . . ? C02 C01 H01 125.5(6) . . . ? C05 C01 H01 124.7(8) . . . ? W1 C02 C01 72.8(5) . . . ? W1 C02 C03 70.5(4) . . . ? W1 C02 H02 120.2(5) . . . ? C01 C02 C03 106.9(5) . . . ? C01 C02 H02 126.7(6) . . . ? C03 C02 H02 126.3(7) . . . ? W1 C03 C02 74.2(4) . . . ? W1 C03 C04 72.3(4) . . . ? W1 C03 H03 120.0(5) . . . ? C02 C03 C04 108.8(6) . . . ? C02 C03 H03 125.8(6) . . . ? C04 C03 H03 125.4(4) . . . ? W1 C04 C03 72.0(3) . . . ? W1 C04 C05 73.4(3) . . . ? W1 C04 H04 120.3(5) . . . ? C03 C04 C05 107.7(4) . . . ? C03 C04 H04 126.7(6) . . . ? C05 C04 H04 125.6(6) . . . ? W1 C05 C01 73.0(4) . . . ? W1 C05 C04 71.1(4) . . . ? W1 C05 H05 122.0(6) . . . ? C01 C05 C04 106.7(7) . . . ? C01 C05 H05 126.2(7) . . . ? C04 C05 H05 127.0(5) . . . ? Cl2 Cl1 C0 17.0(12) . . . ? Cl2 Cl1 H0a 43.7(4) . . . ? Cl2 Cl1 H0b 42.8(3) . . . ? Cl2 Cl1 Cl1 26.7(3) . . 2_676 ? Cl2 Cl1 Cl2 121.8(9) . . 2_676 ? Cl2 Cl1 C0 60.8(13) . . 2_676 ? Cl2 Cl1 H0b 56.1(5) . . 2_676 ? C0 Cl1 H0a 32.6(12) . . . ? C0 Cl1 H0b 29.2(8) . . . ? C0 Cl1 Cl1 29.4(11) . . 2_676 ? C0 Cl1 Cl2 118.2(12) . . 2_676 ? C0 Cl1 C0 66.9(18) . . 2_676 ? C0 Cl1 H0b 72.0(13) . . 2_676 ? H0a Cl1 H0b 47.6(3) . . . ? H0a Cl1 Cl1 61.8(5) . . 2_676 ? H0a Cl1 Cl2 135.3(9) . . 2_676 ? H0a Cl1 C0 99.3(15) . . 2_676 ? H0a Cl1 H0b 97.8(7) . . 2_676 ? H0b Cl1 Cl1 32.5(3) . . 2_676 ? H0b Cl1 Cl2 91.8(7) . . 2_676 ? H0b Cl1 C0 60.2(15) . . 2_676 ? H0b Cl1 H0b 86.3(6) . . 2_676 ? Cl1 Cl1 Cl2 95.1(8) 2_676 . 2_676 ? Cl1 Cl1 C0 37.6(14) 2_676 . 2_676 ? Cl1 Cl1 H0b 53.8(5) 2_676 . 2_676 ? Cl2 Cl1 C0 65.2(13) 2_676 . 2_676 ? Cl2 Cl1 H0b 96.8(9) 2_676 . 2_676 ? C0 Cl1 H0b 43.5(12) 2_676 . 2_676 ? Cl1 Cl2 C0 19.8(13) . . . ? Cl1 Cl2 H0a 42.5(4) . . . ? Cl1 Cl2 H0b 43.5(3) . . . ? Cl1 Cl2 Cl1 58.2(8) . . 2_676 ? Cl1 Cl2 C0 27.0(8) . . 2_676 ? C0 Cl2 H0a 30.2(12) . . . ? C0 Cl2 H0b 28.0(11) . . . ? C0 Cl2 Cl1 57.8(12) . . 2_676 ? C0 Cl2 C0 37.5(15) . . 2_676 ? H0a Cl2 H0b 47.4(3) . . . ? H0a Cl2 Cl1 86.3(8) . . 2_676 ? H0a Cl2 C0 66.8(9) . . 2_676 ? H0b Cl2 Cl1 42.1(6) . . 2_676 ? H0b Cl2 C0 44.0(7) . . 2_676 ? Cl1 Cl2 C0 34.8(9) 2_676 . 2_676 ? Cl1 C0 Cl2 143(2) . . . ? Cl1 C0 H0a 91(2) . . . ? Cl1 C0 H0b 96(2) . . . ? Cl1 C0 Cl1 113.1(19) . . 2_676 ? Cl1 C0 Cl2 27.0(5) . . 2_676 ? Cl1 C0 C0 47.2(16) . . 2_676 ? Cl2 C0 H0a 107.6(19) . . . ? Cl2 C0 H0b 110(3) . . . ? Cl2 C0 Cl1 57.0(16) . . 2_676 ? Cl2 C0 Cl2 142(2) . . 2_676 ? Cl2 C0 C0 111(3) . . 2_676 ? H0a C0 H0b 103(3) . . . ? H0a C0 Cl1 155(3) . . 2_676 ? H0a C0 Cl2 108(2) . . 2_676 ? H0a C0 C0 138(3) . . 2_676 ? H0b C0 Cl1 69.0(18) . . 2_676 ? H0b C0 Cl2 72.3(15) . . 2_676 ? H0b C0 C0 79.7(16) . . 2_676 ? Cl1 C0 Cl2 92.1(13) 2_676 . 2_676 ? Cl1 C0 C0 65.9(19) 2_676 . 2_676 ? Cl2 C0 C0 31.4(14) 2_676 . 2_676 ? Cl1 H0a Cl2 93.8(5) . . . ? Cl1 H0a C0 56.6(18) . . . ? Cl2 H0a C0 42.2(16) . . . ? Cl1 H0b Cl2 93.7(5) . . . ? Cl1 H0b C0 55(2) . . . ? Cl1 H0b Cl1 93.7(6) . . 2_676 ? Cl2 H0b C0 42(2) . . . ? Cl2 H0b Cl1 41.1(5) . . 2_676 ? C0 H0b Cl1 68(2) . . 2_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 13 _reflns_limit_k_min -15 _reflns_limit_k_max 14 _reflns_limit_l_min -16 _reflns_limit_l_max 15 _reflns_number_total 5322 _reflns_number_observed 4442 _reflns_observed_criterion refl_observed_if_F____>4.000_sigma(F___) _reflns_d_resolution_high .73 _reflns_d_resolution_low 10.452 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 4.7759 _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_author ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 _publ_contact_author_fax (61)-8-9380-1005 _publ_contact_author_email bws@crystal.uwa.edu.au loop_ _publ_author_name _publ_author_address '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=END data_br607 _audit_creation_date 98-11-04 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common 'compound 2' _chemical_formula_analytical C30_H10_Co2_O12_W2 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum C30_H10_Co2_O12_W2 _chemical_formula_weight 1047.96 _chemical_melting_point ? _computing_data_collection 'Bruker SMART software' _computing_cell_refinement 'Bruker SMART software' _computing_data_reduction 'Bruker SAINT software' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 6.9570(8) _cell_length_b 12.2800(14) _cell_length_c 18.768(2) _cell_angle_alpha 99.267(2) _cell_angle_beta 96.708(2) _cell_angle_gamma 94.144(2) _cell_volume 1564.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 0 _cell_measurement_theta_max 29 _cell_special_details ; ? ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _exptl_crystal_description bar _exptl_crystal_preparation ? _exptl_crystal_colour dark _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 976 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_coefficient_mu 8.43 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.527 _exptl_absorpt_correction_T_max 0.914 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device 'Bruker CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 18066 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI .042 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 29.18 _diffrn_reflns_reduction_process ? loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 60 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 20 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Co ? 0 4 .299 .973 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 24 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 W ? 0 4 -1.421 6.872 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom W1 .39244(4) .22030(2) -.056401(15) .03804(15) Uani ? ? W1' .95901(4) -.23142(3) .407418(16) .04167(16) Uani ? ? Co2 .13701(14) .19889(8) .24332(5) .0400(5) Uani ? ? Co3 .40505(15) .34756(8) .27196(6) .0407(5) Uani ? ? C11 .3213(15) .3619(8) -.0027(5) .064(5) Uani ? ? O11 .2833(15) .4439(6) .0273(5) .111(6) Uani ? ? C12 .1893(13) .0960(8) -.0599(4) .051(4) Uani ? ? O12 .0833(10) .0194(6) -.0645(4) .073(4) Uani ? ? C13 .1797(13) .2618(7) -.1270(5) .054(4) Uani ? ? O13 .0588(10) .2890(6) -.1661(4) .080(4) Uani ? ? C21 -.0209(12) .2433(8) .1701(5) .056(4) Uani ? ? O21 -.1068(11) .2709(7) .1236(4) .099(5) Uani ? ? C22 .0278(12) .2416(8) .3263(4) .051(4) Uani ? ? O22 -.0389(10) .2740(7) .3758(4) .078(4) Uani ? ? C23 .0705(13) .0520(8) .2319(5) .056(5) Uani ? ? O23 .0387(12) -.0407(6) .2261(4) .085(5) Uani ? ? C31 .2722(13) .4488(7) .2317(5) .055(4) Uani ? ? O31 .1918(10) .5108(6) .2052(5) .089(5) Uani ? ? C32 .4161(14) .3812(7) .3715(5) .062(5) Uani ? ? O32 .4238(13) .3956(8) .4325(4) .105(5) Uani ? ? C33 .6491(14) .4022(7) .2643(5) .060(5) Uani ? ? O33 .7976(11) .4361(7) .2600(6) .106(6) Uani ? ? C1 .3964(11) .2027(6) .0555(4) .043(4) Uani ? ? C2 .3920(11) .2033(6) .1190(4) .042(3) Uani ? ? C3 .3667(11) .2157(6) .1941(4) .040(3) Uani ? ? C4 .4216(11) .1868(6) .2580(4) .036(3) Uani ? ? C101 .7216(13) .2722(10) -.0516(5) .069(5) Uani ? ? C102 .7110(14) .1651(10) -.0419(5) .068(5) Uani ? ? C103 .6085(14) .0983(8) -.1051(6) .068(5) Uani ? ? C104 .5542(14) .1671(9) -.1551(5) .065(5) Uani ? ? C105 .6259(13) .2756(8) -.1213(5) .057(5) Uani ? ? C11' .8173(13) -.1770(7) .4918(5) .052(4) Uani ? ? O11' .7387(11) -.1462(6) .5387(4) .077(4) Uani ? ? C12' .7603(13) -.2983(7) .3240(5) .056(4) Uani ? ? O12' .6435(10) -.3344(6) .2759(4) .073(4) Uani ? ? C13' .8671(14) -.3751(7) .4343(5) .059(5) Uani ? ? O13' .8194(12) -.4595(6) .4489(4) .092(5) Uani ? ? C1' .8116(11) -.0990(6) .3748(4) .043(4) Uani ? ? C2' .7216(11) -.0272(6) .3505(4) .043(4) Uani ? ? C3' .6202(11) .0489(6) .3213(4) .041(3) Uani ? ? C4' .5314(11) .1141(6) .2920(4) .040(3) Uani ? ? C101' 1.2618(14) -.1372(11) .4595(6) .081(6) Uani ? ? C102' 1.2360(14) -.1208(9) .3880(6) .066(5) Uani ? ? C103' 1.2249(14) -.2229(9) .3427(5) .065(5) Uani ? ? C104' 1.2472(15) -.3056(10) .3849(7) .080(6) Uani ? ? C105' 1.2704(14) -.2498(11) .4595(6) .081(7) Uani ? ? H101 .78237 .33508 -.01634 .08800 Uiso ? ? H102 .76608 .13838 .00082 .08400 Uiso ? ? H103 .57813 .01824 -.11214 .08400 Uiso ? ? H104 .47988 .14319 -.20330 .08200 Uiso ? ? H105 .61031 .34139 -.14313 .07000 Uiso ? ? H101' 1.27061 -.08019 .50299 .10000 Uiso ? ? H102' 1.22710 -.04908 .37230 .08400 Uiso ? ? H103' 1.20605 -.23515 .28996 .08100 Uiso ? ? H104' 1.24685 -.38426 .36818 .09900 Uiso ? ? H105' 1.28907 -.28510 .50150 .10100 Uiso ? ? 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 W1 .04676(19) .03939(17) .03069(16) .00893(13) .00910(12) .00901(12) W1' .04489(19) .0456(2) .03644(18) .01502(14) .00105(13) .01107(13) Co2 .0408(5) .0478(6) .0313(5) .0080(4) .0015(4) .0072(4) Co3 .0476(6) .0376(5) .0369(5) .0080(4) .0037(4) .0061(4) C11 .083(7) .053(5) .059(6) .012(5) .018(5) .013(4) O11 .182(9) .060(5) .102(7) .038(5) .057(6) .001(4) C12 .058(5) .067(6) .032(4) .006(4) .007(4) .020(4) O12 .072(4) .084(5) .065(5) -.016(4) .004(3) .029(4) C13 .057(5) .059(5) .049(5) .013(4) .009(4) .019(4) O13 .071(5) .105(6) .072(5) .024(4) -.002(4) .044(4) C21 .052(5) .073(6) .041(5) .017(4) -.003(4) .007(4) O21 .091(6) .129(7) .068(5) .029(5) -.036(4) .012(5) C22 .045(4) .067(6) .039(5) .007(4) .006(4) .007(4) O22 .074(5) .115(6) .042(4) .012(4) .014(3) -.001(4) C23 .058(5) .066(6) .043(5) -.003(4) .007(4) .011(4) O23 .120(6) .056(4) .076(5) -.010(4) .022(4) .007(4) C31 .059(5) .044(5) .068(6) .012(4) .012(4) .017(4) O31 .085(5) .069(5) .123(7) .024(4) .004(5) .047(5) C32 .075(6) .057(5) .047(5) -.014(4) .005(4) .001(4) O32 .125(7) .133(8) .045(4) -.023(6) .008(4) -.005(4) C33 .059(6) .052(5) .071(6) .015(4) .018(5) .007(4) O33 .061(5) .079(5) .180(10) -.001(4) .042(5) .008(6) C1 .054(5) .043(4) .033(4) .009(3) .012(3) .007(3) C2 .048(4) .040(4) .038(4) .010(3) .009(3) .006(3) C3 .048(4) .037(4) .036(4) .012(3) .004(3) .004(3) C4 .050(4) .031(3) .029(3) .005(3) .006(3) .006(3) C101 .048(5) .121(9) .039(5) .011(5) .008(4) .014(5) C102 .061(6) .095(8) .055(6) .044(6) .008(4) .012(5) C103 .066(6) .057(6) .085(7) .030(5) .029(5) .002(5) C104 .061(6) .093(8) .045(5) .023(5) .018(4) .004(5) C105 .057(5) .070(6) .051(5) .005(4) .022(4) .023(4) C11' .053(5) .054(5) .050(5) .013(4) .001(4) .015(4) O11' .089(5) .089(5) .063(4) .029(4) .030(4) .016(4) C12' .059(5) .049(5) .059(6) .011(4) -.003(4) .012(4) O12' .075(5) .071(4) .063(4) -.001(4) -.016(4) .004(3) C13' .074(6) .044(5) .055(5) .004(4) .002(4) .004(4) O13' .123(7) .064(5) .093(6) -.001(4) .017(5) .029(4) C1' .048(4) .042(4) .039(4) .007(3) .001(3) .008(3) C2' .043(4) .047(4) .041(4) .009(3) .001(3) .010(3) C3' .042(4) .045(4) .036(4) .006(3) .004(3) .010(3) C4' .048(4) .038(4) .035(4) .007(3) .004(3) .004(3) C101' .052(6) .110(9) .068(7) .014(6) -.014(5) -.006(6) C102' .052(5) .081(7) .066(6) .005(5) .009(5) .018(5) C103' .068(6) .085(7) .040(5) .003(5) .014(4) .006(5) C104' .055(6) .086(8) .107(9) .032(5) .027(6) .016(7) C105' .048(5) .125(10) .077(8) .027(6) -.013(5) .047(7) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 6299 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .059 _refine_ls_R_factor_obs .048 _refine_ls_wR_factor_all .057 _refine_ls_wR_factor_obs .056 _refine_ls_goodness_of_fit_all 1.719 _refine_ls_goodness_of_fit_obs 1.847 _refine_ls_shift/esd_max .075 _refine_ls_shift/esd_mean .002 _refine_diff_density_min -2.775 _refine_diff_density_max 2.907 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C11 1.990(10) . . ? W1 C12 1.992(9) . . ? W1 C13 2.019(9) . . ? W1 C1 2.143(8) . . ? W1 C101 2.320(9) . . ? W1 C102 2.362(10) . . ? W1 C103 2.354(10) . . ? W1 C104 2.308(10) . . ? W1 C105 2.269(10) . . ? W1' C11' 2.011(9) . . ? W1' C12' 1.988(8) . . ? W1' C13' 1.994(10) . . ? W1' C1' 2.118(8) . . ? W1' C101' 2.352(10) . . ? W1' C102' 2.374(10) . . ? W1' C103' 2.334(10) . . ? W1' C104' 2.316(11) . . ? W1' C105' 2.312(10) . . ? Co2 Co3 2.4611(14) . . ? Co2 C21 1.835(9) . . ? Co2 C22 1.830(9) . . ? Co2 C23 1.802(10) . . ? Co2 C3 1.951(8) . . ? Co2 C4 1.987(7) . . ? Co3 C31 1.810(9) . . ? Co3 C32 1.838(9) . . ? Co3 C33 1.810(10) . . ? Co3 C3 1.978(7) . . ? Co3 C4 1.963(7) . . ? C11 O11 1.136(13) . . ? C12 O12 1.137(11) . . ? C13 O13 1.155(12) . . ? C21 O21 1.112(12) . . ? C22 O22 1.116(11) . . ? C23 O23 1.129(12) . . ? C31 O31 1.123(12) . . ? C32 O32 1.124(12) . . ? C33 O33 1.102(13) . . ? C1 C2 1.194(11) . . ? C2 C3 1.426(11) . . ? C3 C4 1.328(10) . . ? C4 C4' 1.397(11) . . ? C101 C102 1.353(18) . . ? C101 C105 1.406(13) . . ? C101 H101 .967(10) . . ? C102 C103 1.411(13) . . ? C102 H102 .964(11) . . ? C103 C104 1.397(16) . . ? C103 H103 .975(9) . . ? C104 C105 1.408(13) . . ? C104 H104 .978(9) . . ? C105 H105 .971(10) . . ? C11' O11' 1.118(12) . . ? C12' O12' 1.148(10) . . ? C13' O13' 1.150(12) . . ? C1' C2' 1.232(11) . . ? C2' C3' 1.357(11) . . ? C3' C4' 1.209(11) . . ? C101' C102' 1.381(16) . . ? C101' C105' 1.39(2) . . ? C101' H101' .979(11) . . ? C102' C103' 1.388(14) . . ? C102' H102' .977(12) . . ? C103' C104' 1.391(18) . . ? C103' H103' .969(9) . . ? C104' C105' 1.442(17) . . ? C104' H104' .967(12) . . ? C105' H105' .959(13) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W1 O11 3.126(8) . . ? W1 O12 3.126(7) . . ? W1 O13 3.173(7) . . ? W1 C2 3.332(8) . . ? W1 H101 2.9224(4) . . ? W1 H102 2.9993(4) . . ? W1 H103 2.9771(4) . . ? W1 H104 2.9158(4) . . ? W1 H105 2.8615(4) . . ? W1' O11' 3.129(8) . . ? W1' O12' 3.136(6) . . ? W1' O13' 3.143(8) . . ? W1' C2' 3.347(8) . . ? W1' H101' 2.9669(3) . . ? W1' H102' 3.0143(4) . . ? W1' H103' 2.9461(4) . . ? W1' H104' 2.9185(4) . . ? W1' H105' 2.9106(4) . . ? Co2 O21 2.945(8) . . ? Co2 O22 2.943(7) . . ? Co2 O23 2.929(7) . . ? Co2 C31 3.193(9) . . ? Co2 C2 3.097(8) . . ? Co2 C4' 3.095(8) . . ? Co3 C22 3.191(9) . . ? Co3 O31 2.932(8) . . ? Co3 O32 2.961(8) . . ? Co3 O33 2.913(8) . . ? Co3 C2 3.110(7) . . ? Co3 C4' 3.125(8) . . ? C11 C13 2.507(12) . . ? C11 C1 2.448(13) . . ? C12 C13 2.562(14) . . ? C12 C1 2.563(10) . . ? O12 O12 2.894(10) . 2 ? O12 H102 2.650(8) . 2_655 ? C13 C104 2.997(14) . . ? C21 C22 2.914(12) . . ? C21 C23 2.861(14) . . ? C21 C3 2.736(12) . . ? O21 H102 2.617(7) . 1_455 ? C22 C23 2.747(12) . . ? C23 C3 2.999(12) . . ? C23 C4 2.797(11) . . ? C31 C32 2.963(14) . . ? C31 C33 2.744(13) . . ? C31 C3 2.975(11) . . ? O31 H105 2.691(8) . 2_665 ? C32 C33 2.759(15) . . ? C32 C4 2.938(11) . . ? O32 O13' 2.990(12) . 2_656 ? C33 C3 2.935(11) . . ? C33 C4 2.961(11) . . ? C1 C3 2.613(11) . . ? C2 C4 2.636(11) . . ? C3 C4' 2.588(11) . . ? C4 C3' 2.605(11) . . ? C101 C103 2.251(14) . . ? C101 C104 2.289(12) . . ? C101 H102 2.070(12) . . ? C101 H105 2.128(11) . . ? C102 C104 2.275(13) . . ? C102 C105 2.229(15) . . ? C102 H101 2.075(11) . . ? C102 H103 2.134(10) . . ? C103 C105 2.242(14) . . ? C103 H102 2.120(10) . . ? C103 H104 2.124(11) . . ? C104 H103 2.122(12) . . ? C104 H105 2.119(11) . . ? C105 H101 2.126(8) . . ? C105 H104 2.153(8) . . ? C11' C13' 2.563(12) . . ? C11' C1' 2.531(13) . . ? O11' H102' 2.671(7) . 2_756 ? C12' C13' 2.469(14) . . ? C12' C1' 2.463(11) . . ? C1' C3' 2.589(11) . . ? C1' C102' 2.969(12) . . ? C2' C4' 2.565(11) . . ? C101' C103' 2.250(14) . . ? C101' C104' 2.291(17) . . ? C101' H102' 2.103(13) . . ? C101' H105' 2.105(14) . . ? C102' C104' 2.267(16) . . ? C102' C105' 2.243(18) . . ? C102' H101' 2.116(10) . . ? C102' H103' 2.107(10) . . ? C103' C105' 2.259(16) . . ? C103' H102' 2.115(11) . . ? C103' H104' 2.124(11) . . ? C104' H103' 2.102(14) . . ? C104' H105' 2.145(14) . . ? C105' H101' 2.111(13) . . ? C105' H104' 2.162(12) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 W1 C12 111.8(4) . . . ? C11 W1 C13 77.4(4) . . . ? C11 W1 C1 72.5(4) . . . ? C11 W1 C101 97.4(4) . . . ? C11 W1 C102 122.3(4) . . . ? C11 W1 C103 154.9(4) . . . ? C11 W1 C104 136.6(4) . . . ? C11 W1 C105 103.6(4) . . . ? C12 W1 C13 79.4(4) . . . ? C12 W1 C1 76.5(3) . . . ? C12 W1 C101 146.1(4) . . . ? C12 W1 C102 112.7(4) . . . ? C12 W1 C103 91.8(4) . . . ? C12 W1 C104 104.8(3) . . . ? C12 W1 C105 140.4(3) . . . ? C13 W1 C1 130.5(3) . . . ? C13 W1 C101 125.2(4) . . . ? C13 W1 C102 145.2(4) . . . ? C13 W1 C103 117.1(4) . . . ? C13 W1 C104 87.4(4) . . . ? C13 W1 C105 91.8(4) . . . ? C1 W1 C101 97.2(3) . . . ? C1 W1 C102 84.2(3) . . . ? C1 W1 C103 106.3(3) . . . ? C1 W1 C104 140.4(3) . . . ? C1 W1 C105 132.8(3) . . . ? C101 W1 C102 33.6(4) . . . ? C101 W1 C103 57.6(4) . . . ? C101 W1 C104 59.3(3) . . . ? C101 W1 C105 35.6(3) . . . ? C102 W1 C103 34.8(3) . . . ? C102 W1 C104 58.3(3) . . . ? C102 W1 C105 57.5(4) . . . ? C103 W1 C104 34.9(4) . . . ? C103 W1 C105 58.0(4) . . . ? C104 W1 C105 35.8(3) . . . ? C11' W1' C12' 107.5(4) . . . ? C11' W1' C13' 79.6(4) . . . ? C11' W1' C1' 75.6(3) . . . ? C11' W1' C101' 95.5(4) . . . ? C11' W1' C102' 118.4(3) . . . ? C11' W1' C103' 151.8(3) . . . ? C11' W1' C104' 139.8(4) . . . ? C11' W1' C105' 104.9(4) . . . ? C12' W1' C13' 76.6(4) . . . ? C12' W1' C1' 73.6(3) . . . ? C12' W1' C101' 153.6(4) . . . ? C12' W1' C102' 120.2(4) . . . ? C12' W1' C103' 97.6(4) . . . ? C12' W1' C104' 106.7(4) . . . ? C12' W1' C105' 141.7(4) . . . ? C13' W1' C1' 132.8(4) . . . ? C13' W1' C101' 121.4(4) . . . ? C13' W1' C102' 144.6(4) . . . ? C13' W1' C103' 119.5(4) . . . ? C13' W1' C104' 88.4(4) . . . ? C13' W1' C105' 89.8(4) . . . ? C1' W1' C101' 100.6(4) . . . ? C1' W1' C102' 82.5(3) . . . ? C1' W1' C103' 100.2(4) . . . ? C1' W1' C104' 135.0(4) . . . ? C1' W1' C105' 135.0(4) . . . ? C101' W1' C102' 34.0(4) . . . ? C101' W1' C103' 57.4(3) . . . ? C101' W1' C104' 58.8(4) . . . ? C101' W1' C105' 34.6(5) . . . ? C102' W1' C103' 34.3(3) . . . ? C102' W1' C104' 57.8(4) . . . ? C102' W1' C105' 57.2(4) . . . ? C103' W1' C104' 34.8(4) . . . ? C103' W1' C105' 58.2(4) . . . ? C104' W1' C105' 36.3(4) . . . ? Co3 Co2 C21 102.7(3) . . . ? Co3 Co2 C22 94.9(3) . . . ? Co3 Co2 C23 145.9(3) . . . ? Co3 Co2 C3 51.7(2) . . . ? Co3 Co2 C4 51.0(2) . . . ? C21 Co2 C22 105.3(4) . . . ? C21 Co2 C23 103.8(4) . . . ? C21 Co2 C3 92.5(4) . . . ? C21 Co2 C4 131.8(4) . . . ? C22 Co2 C23 98.3(4) . . . ? C22 Co2 C3 145.4(3) . . . ? C22 Co2 C4 115.4(3) . . . ? C23 Co2 C3 106.0(4) . . . ? C23 Co2 C4 95.0(4) . . . ? C3 Co2 C4 39.4(3) . . . ? Co2 Co3 C31 95.6(3) . . . ? Co2 Co3 C32 100.7(3) . . . ? Co2 Co3 C33 151.3(3) . . . ? Co2 Co3 C3 50.7(2) . . . ? Co2 Co3 C4 51.9(2) . . . ? C31 Co3 C32 108.6(4) . . . ? C31 Co3 C33 98.6(4) . . . ? C31 Co3 C3 103.4(3) . . . ? C31 Co3 C4 139.8(3) . . . ? C32 Co3 C33 98.3(4) . . . ? C32 Co3 C3 139.1(4) . . . ? C32 Co3 C4 101.2(4) . . . ? C33 Co3 C3 101.5(4) . . . ? C33 Co3 C4 103.3(4) . . . ? C3 Co3 C4 39.4(3) . . . ? W1 C11 O11 178.6(10) . . . ? W1 C12 O12 174.4(8) . . . ? W1 C13 O13 177.8(7) . . . ? Co2 C21 O21 175.7(9) . . . ? Co2 C22 O22 175.7(9) . . . ? Co2 C23 O23 176.3(8) . . . ? Co3 C31 O31 178.2(9) . . . ? Co3 C32 O32 176.0(9) . . . ? Co3 C33 O33 179.5(9) . . . ? W1 C1 C2 173.4(7) . . . ? C1 C2 C3 171.6(8) . . . ? Co2 C3 Co3 77.6(3) . . . ? Co2 C3 C2 132.3(5) . . . ? Co2 C3 C4 71.7(5) . . . ? Co3 C3 C2 131.3(6) . . . ? Co3 C3 C4 69.7(4) . . . ? C2 C3 C4 146.2(8) . . . ? Co2 C4 Co3 77.1(3) . . . ? Co2 C4 C3 68.9(5) . . . ? Co2 C4 C4' 131.5(6) . . . ? Co3 C4 C3 70.9(4) . . . ? Co3 C4 C4' 136.2(5) . . . ? C3 C4 C4' 143.5(7) . . . ? W1 C101 C102 74.9(6) . . . ? W1 C101 C105 70.2(5) . . . ? W1 C101 H101 119.7(7) . . . ? C102 C101 C105 107.8(9) . . . ? C102 C101 H101 126.0(10) . . . ? C105 C101 H101 126.2(12) . . . ? W1 C102 C101 71.5(6) . . . ? W1 C102 C103 72.3(6) . . . ? W1 C102 H102 123.1(8) . . . ? C101 C102 C103 109.0(9) . . . ? C101 C102 H102 125.7(9) . . . ? C103 C102 H102 125.3(11) . . . ? W1 C103 C102 72.9(6) . . . ? W1 C103 C104 70.7(6) . . . ? W1 C103 H103 121.1(8) . . . ? C102 C103 C104 108.2(9) . . . ? C102 C103 H103 125.8(11) . . . ? C104 C103 H103 126.0(10) . . . ? W1 C104 C103 74.4(6) . . . ? W1 C104 C105 70.6(6) . . . ? W1 C104 H104 119.5(7) . . . ? C103 C104 C105 106.1(8) . . . ? C103 C104 H104 126.0(11) . . . ? C105 C104 H104 127.9(11) . . . ? W1 C105 C101 74.1(6) . . . ? W1 C105 C104 73.6(6) . . . ? W1 C105 H105 118.4(7) . . . ? C101 C105 C104 108.9(9) . . . ? C101 C105 H105 126.2(9) . . . ? C104 C105 H105 124.9(9) . . . ? W1' C11' O11' 179.6(8) . . . ? W1' C12' O12' 178.2(8) . . . ? W1' C13' O13' 177.7(9) . . . ? W1' C1' C2' 175.0(6) . . . ? C1' C2' C3' 177.7(7) . . . ? C2' C3' C4' 176.8(8) . . . ? C4 C4' C3' 177.7(8) . . . ? W1' C101' C102' 73.9(6) . . . ? W1' C101' C105' 71.1(6) . . . ? W1' C101' H101' 120.1(8) . . . ? C102' C101' C105' 108.2(10) . . . ? C102' C101' H101' 126.5(13) . . . ? C105' C101' H101' 125.3(12) . . . ? W1' C102' C101' 72.1(6) . . . ? W1' C102' C103' 71.3(6) . . . ? W1' C102' H102' 122.5(7) . . . ? C101' C102' C103' 108.7(10) . . . ? C101' C102' H102' 125.4(10) . . . ? C103' C102' H102' 126.0(10) . . . ? W1' C103' C102' 74.5(6) . . . ? W1' C103' C104' 71.9(6) . . . ? W1' C103' H103' 120.5(7) . . . ? C102' C103' C104' 109.3(9) . . . ? C102' C103' H103' 125.8(11) . . . ? C104' C103' H103' 124.9(11) . . . ? W1' C104' C103' 73.3(6) . . . ? W1' C104' C105' 71.7(6) . . . ? W1' C104' H104' 119.7(8) . . . ? C103' C104' C105' 105.7(10) . . . ? C103' C104' H104' 127.6(13) . . . ? C105' C104' H104' 126.6(14) . . . ? W1' C105' C101' 74.3(6) . . . ? W1' C105' C104' 72.0(6) . . . ? W1' C105' H105' 119.8(8) . . . ? C101' C105' C104' 108.1(11) . . . ? C101' C105' H105' 126.5(11) . . . ? C104' C105' H105' 125.4(13) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min -25 _reflns_limit_l_max 25 _reflns_number_total 7621 _reflns_number_observed 6299 _reflns_observed_criterion refl_observed_if_F____>4.000_sigma(F___) _reflns_d_resolution_high .729 _reflns_d_resolution_low 18.297 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 12.8938 _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_author ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 _publ_contact_author_fax (61)-8-9380-1005 _publ_contact_author_email bws@crystal.uwa.edu.au loop_ _publ_author_name _publ_author_address '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=END data_br601 _audit_creation_date 98-08-21 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common 'compound 5' _chemical_formula_analytical C84_H58_Cl4_Co4_O14_P2_W2 _chemical_formula_moiety ? _chemical_formula_structural C82_H54_Co4_O14_P2_W2.2CH2Cl2 _chemical_formula_sum C84_H58_Cl4_Co4_O14_P2_W2 _chemical_formula_weight 2160.51 _chemical_melting_point ? _computing_data_collection 'Bruker SMART software' _computing_cell_refinement 'Bruker SAINT software' _computing_data_reduction 'Bruker SAINT software' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 19.256(2) _cell_length_b 14.656(2) _cell_length_c 30.558(4) _cell_angle_alpha 90.00000 _cell_angle_beta 105.234(2) _cell_angle_gamma 90.00000 _cell_volume 8320.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 6298 _cell_measurement_theta_min 0 _cell_measurement_theta_max 29 _cell_special_details ; ? ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description cuboid _exptl_crystal_preparation ? _exptl_crystal_colour dark _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 4232 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_coefficient_mu 3.80 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.888 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device 'Bruker area detector diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 44221 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI .066 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 29.18 _diffrn_reflns_reduction_process ? loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 336 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 232 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 16 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 56 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 16 .09 .095 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Co ? 0 16 .299 .973 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 W ? 0 8 -1.421 6.872 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom W1 .650728(10) .375316(12) .437042(6) .05173(10) Uani ? ? Co2 .74159(3) .54155(3) .372268(16) .0405(2) Uani ? ? Co3 .62217(3) .60665(3) .367711(16) .0403(2) Uani ? ? C11 .6529(3) .3332(4) .49889(17) .080(3) Uani ? ? O11 .6547(3) .3087(3) .53503(13) .112(3) Uani ? ? C12 .5840(3) .4603(4) .45404(18) .076(3) Uani ? ? O12 .5413(3) .5080(3) .46304(17) .122(3) Uani ? ? C13 .7487(3) .4120(3) .47360(16) .068(3) Uani ? ? O13 .8040(2) .4319(3) .49427(13) .096(2) Uani ? ? C21 .7078(2) .5100(3) .31533(14) .055(2) Uani ? ? O21 .6850(2) .4868(3) .27805(11) .083(2) Uani ? ? C22 .8075(2) .4553(3) .39011(14) .053(2) Uani ? ? O22 .8479(2) .3977(2) .40063(13) .083(2) Uani ? ? C31 .5617(2) .5405(3) .32512(13) .051(2) Uani ? ? O31 .52022(18) .4961(2) .30080(11) .078(2) Uani ? ? C32 .5572(2) .6551(3) .39298(14) .056(2) Uani ? ? O32 .5140(2) .6868(3) .40724(11) .083(2) Uani ? ? C1 .6749(2) .5081(3) .40986(11) .0406(17) Uani ? ? C2 .7048(2) .5910(3) .42176(12) .0394(17) Uani ? ? C3 .7259(2) .6523(3) .45786(12) .0419(18) Uani ? ? C4 .7413(2) .7149(3) .48466(12) .0443(19) Uani ? ? P1 .80583(5) .66639(7) .36986(3) .0427(5) Uani ? ? C111 .8464(2) .6835(3) .32255(14) .050(2) Uani ? ? C112 .8482(3) .6130(3) .29308(18) .071(3) Uani ? ? C113 .8767(4) .6249(5) .2562(2) .095(4) Uani ? ? C114 .9029(3) .7066(6) .2483(2) .094(4) Uani ? ? C115 .9039(3) .7775(5) .2775(2) .089(4) Uani ? ? C116 .8758(3) .7662(4) .31490(18) .075(3) Uani ? ? C121 .8813(2) .6868(3) .41992(13) .049(2) Uani ? ? C122 .8937(2) .7686(4) .44334(17) .069(3) Uani ? ? C123 .9494(3) .7762(4) .48324(18) .084(3) Uani ? ? C124 .9921(3) .7051(5) .49863(17) .082(3) Uani ? ? C125 .9831(3) .6243(4) .4762(2) .081(3) Uani ? ? C126 .9274(3) .6153(3) .43679(18) .067(3) Uani ? ? C0 .7479(2) .7659(3) .36830(13) .047(2) Uani ? ? P2 .65361(5) .73751(7) .33989(3) .0422(5) Uani ? ? C211 .6479(2) .7463(3) .27913(13) .047(2) Uani ? ? C212 .6865(3) .8098(4) .26172(16) .076(3) Uani ? ? C213 .6762(3) .8182(4) .21591(19) .095(4) Uani ? ? C214 .6267(3) .7670(4) .18668(17) .089(4) Uani ? ? C215 .5889(4) .7035(4) .20320(17) .102(4) Uani ? ? C216 .5995(3) .6932(4) .24939(15) .073(3) Uani ? ? C221 .6078(2) .8417(3) .35008(15) .052(2) Uani ? ? C222 .6151(3) .8699(3) .39441(19) .076(3) Uani ? ? C223 .5806(4) .9485(5) .4032(2) .101(4) Uani ? ? C224 .5390(4) .9989(4) .3681(3) .106(5) Uani ? ? C225 .5303(4) .9714(4) .3251(3) .106(4) Uani ? ? C226 .5650(3) .8930(4) .3152(2) .082(3) Uani ? ? C01 .6343(3) .3272(3) .36101(16) .071(3) Uani ? ? C02 .5705(3) .3174(4) .37144(18) .076(3) Uani ? ? C03 .5783(4) .2528(4) .4064(2) .088(4) Uani ? ? C04 .6513(4) .2237(3) .4169(2) .096(4) Uani ? ? C05 .6840(3) .2719(4) .3873(2) .085(3) Uani ? ? Cl11 .7599(4) .4701(4) .6367(4) .213(7) Uani ? ? Cl12 .6139(4) .5013(5) .6351(5) .209(7) Uani ? ? C110 .6902(17) .4930(9) .6714(4) .138(14) Uani ? ? Cl21 .7158(5) .4974(5) .5836(4) .168(6) Uani ? ? Cl22 .6866(16) .4485(16) .6463(11) .44(3) Uani ? ? C210 .6312(17) .475(2) .6021(10) .17(2) Uani ? ? H112 .82948 .55383 .29864 .08700 Uiso ? ? H113 .87843 .57564 .23552 .11300 Uiso ? ? H114 .92125 .71644 .22236 .11100 Uiso ? ? H115 .92472 .83663 .27291 .10500 Uiso ? ? H116 .87675 .81700 .33570 .09100 Uiso ? ? H122 .86258 .82019 .43174 .08300 Uiso ? ? H123 .95776 .83356 .49898 .09900 Uiso ? ? H124 1.02959 .71089 .52668 .09700 Uiso ? ? H125 1.01468 .57360 .48754 .09700 Uiso ? ? H126 .92019 .55777 .42058 .07900 Uiso ? ? H0a .76329 .81431 .35184 .05400 Uiso ? ? H0b .75106 .78640 .39822 .05400 Uiso ? ? H212 .72086 .84767 .28256 .08900 Uiso ? ? H213 .70568 .86099 .20390 .10600 Uiso ? ? H214 .61784 .77478 .15426 .10400 Uiso ? ? H215 .55482 .66488 .18240 .11700 Uiso ? ? H216 .57238 .64719 .26077 .08700 Uiso ? ? H222 .64429 .83346 .41939 .09300 Uiso ? ? H223 .58750 .96980 .43449 .11900 Uiso ? ? H224 .51641 1.05446 .37397 .12600 Uiso ? ? H225 .50021 1.00650 .29948 .12400 Uiso ? ? H226 .55926 .87351 .28385 .09700 Uiso ? ? H01 .64199 .36645 .33754 .08700 Uiso ? ? H02 .52606 .35054 .35797 .09300 Uiso ? ? H03 .54246 .23136 .42027 .10800 Uiso ? ? H04 .67453 .17897 .43937 .11500 Uiso ? ? H05 .73456 .26605 .38651 .10200 Uiso ? ? H110a .70136 .43428 .69156 .03800 Uiso ? ? H110b .71320 .53897 .69144 .03800 Uiso ? ? H210a .61029 .52389 .60171 .03800 Uiso ? ? H210b .60657 .43225 .57580 .03800 Uiso ? ? 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 W1 .06565(12) .04492(10) .04169(10) -.01281(8) .00892(8) .00252(7) Co2 .0476(3) .0375(3) .0362(3) -.0014(2) .0110(2) -.0056(2) Co3 .0442(3) .0420(3) .0337(3) -.0038(2) .0087(2) -.0034(2) C11 .096(4) .086(4) .050(3) -.032(3) .006(3) .011(3) O11 .139(4) .132(4) .059(2) -.048(3) .016(2) .023(2) C12 .099(4) .068(3) .070(3) -.018(3) .040(3) .006(3) O12 .164(4) .093(3) .150(4) .020(3) .113(4) .016(3) C13 .085(4) .065(3) .046(3) -.016(3) .003(2) .017(2) O13 .087(3) .108(3) .072(2) -.029(2) -.017(2) .022(2) C21 .055(3) .061(3) .049(2) .003(2) .015(2) -.010(2) O21 .084(2) .112(3) .0479(19) .010(2) .0087(17) -.027(2) C22 .060(3) .048(2) .052(2) .006(2) .016(2) -.003(2) O22 .088(3) .067(2) .089(3) .023(2) .015(2) .007(2) C31 .059(3) .050(2) .041(2) -.002(2) .008(2) -.0012(18) O31 .079(2) .080(2) .060(2) -.022(2) -.0093(17) -.0110(18) C32 .058(3) .067(3) .041(2) -.001(2) .013(2) -.002(2) O32 .078(2) .112(3) .068(2) .023(2) .033(2) -.009(2) C1 .048(2) .043(2) .0288(17) -.0024(17) .0076(15) -.0021(15) C2 .042(2) .041(2) .0343(18) -.0018(16) .0087(16) -.0022(16) C3 .045(2) .044(2) .036(2) -.0039(17) .0100(16) -.0021(16) C4 .045(2) .052(2) .0346(19) -.0026(18) .0080(16) -.0062(17) P1 .0452(6) .0432(5) .0402(5) -.0034(4) .0120(4) -.0024(4) C111 .044(2) .059(3) .050(2) -.0007(19) .0163(18) .007(2) C112 .076(3) .078(3) .071(3) -.008(3) .038(3) -.006(3) C113 .106(5) .119(6) .075(4) .002(4) .050(4) -.010(4) C114 .077(4) .148(6) .063(3) .004(4) .032(3) .026(4) C115 .079(4) .110(5) .083(4) -.017(3) .032(3) .031(4) C116 .074(3) .085(4) .074(3) -.017(3) .033(3) -.000(3) C121 .046(2) .058(2) .044(2) -.004(2) .0144(18) .0014(19) C122 .059(3) .076(3) .065(3) .003(2) .004(2) -.020(3) C123 .072(3) .108(5) .064(3) .001(3) .006(3) -.035(3) C124 .066(3) .125(5) .051(3) -.016(3) .006(2) .006(3) C125 .061(3) .087(4) .082(4) -.012(3) -.005(3) .031(3) C126 .057(3) .057(3) .078(3) -.008(2) -.000(2) .009(2) C0 .048(2) .040(2) .050(2) -.0045(17) .0080(18) -.0056(17) P2 .0463(5) .0384(5) .0404(5) -.0009(4) .0088(4) -.0016(4) C211 .048(2) .046(2) .043(2) -.0019(18) .0083(17) .0038(17) C212 .083(3) .085(4) .055(3) -.033(3) .010(3) .005(3) C213 .104(4) .110(5) .066(3) -.050(4) .011(3) .029(3) C214 .121(5) .099(4) .046(3) -.039(4) .018(3) .010(3) C215 .137(5) .110(5) .047(3) -.073(4) .002(3) .001(3) C216 .086(3) .087(4) .042(2) -.041(3) .009(2) .007(2) C221 .051(2) .043(2) .062(3) .0038(18) .014(2) -.004(2) C222 .087(4) .070(3) .072(3) .019(3) .023(3) -.010(3) C223 .105(5) .093(5) .115(5) .005(4) .044(4) -.042(4) C224 .119(5) .063(4) .141(6) .025(4) .046(5) -.009(4) C225 .110(5) .080(4) .132(6) .045(4) .035(5) .021(4) C226 .090(4) .068(3) .085(4) .023(3) .018(3) .006(3) C01 .112(5) .048(3) .053(3) -.019(3) .021(3) -.010(2) C02 .083(4) .070(3) .064(3) -.020(3) .001(3) -.014(3) C03 .115(5) .075(4) .083(4) -.055(4) .039(4) -.025(3) C04 .157(7) .041(3) .077(4) .004(3) .004(4) .006(3) C05 .092(4) .070(4) .090(4) -.008(3) .020(3) -.027(3) Cl11 .182(6) .126(4) .352(15) -.011(4) .104(7) -.017(5) Cl12 .181(6) .143(5) .338(13) -.014(4) .129(8) -.018(6) C110 .31(3) .050(6) .062(7) -.059(11) .068(11) -.027(5) Cl21 .184(7) .111(4) .233(10) -.034(4) .099(7) -.077(5) Cl22 .48(4) .34(2) .57(4) -.05(3) .28(4) .15(2) C210 .13(2) .14(2) .18(2) -.009(16) -.03(2) -.09(2) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 7746 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .055 _refine_ls_R_factor_obs .034 _refine_ls_wR_factor_all .044 _refine_ls_wR_factor_obs .041 _refine_ls_goodness_of_fit_all 1.165 _refine_ls_goodness_of_fit_obs 1.266 _refine_ls_shift/esd_max .073 _refine_ls_shift/esd_mean .002 _refine_diff_density_min -1.23 _refine_diff_density_max 1.936 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C11 1.978(5) . . ? W1 C12 1.955(6) . . ? W1 C13 1.997(5) . . ? W1 C1 2.213(4) . . ? W1 C01 2.368(5) . . ? W1 C02 2.345(5) . . ? W1 C03 2.314(6) . . ? W1 C04 2.307(5) . . ? W1 C05 2.350(7) . . ? Co2 Co3 2.4595(8) . . ? Co2 C21 1.752(4) . . ? Co2 C22 1.772(4) . . ? Co2 C1 1.996(4) . . ? Co2 C2 1.969(4) . . ? Co2 P1 2.2206(12) . . ? Co3 C31 1.787(4) . . ? Co3 C32 1.781(5) . . ? Co3 C1 2.022(3) . . ? Co3 C2 1.983(3) . . ? Co3 P2 2.2444(12) . . ? C11 O11 1.153(7) . . ? C12 O12 1.166(8) . . ? C13 O13 1.125(6) . . ? C21 O21 1.159(5) . . ? C22 O22 1.137(6) . . ? C31 O31 1.141(5) . . ? C32 O32 1.135(6) . . ? C1 C2 1.353(5) . . ? C2 C3 1.398(5) . . ? C3 C4 1.214(5) . . ? C4 C4 1.372(5) . 7_666 ? P1 C111 1.832(5) . . ? P1 C121 1.837(4) . . ? P1 C0 1.830(4) . . ? C111 C112 1.377(7) . . ? C111 C116 1.384(7) . . ? C112 C113 1.386(10) . . ? C112 H112 .972(5) . . ? C113 C114 1.347(11) . . ? C113 H113 .966(7) . . ? C114 C115 1.365(10) . . ? C114 H114 .961(7) . . ? C115 C116 1.397(9) . . ? C115 H115 .980(7) . . ? C116 H116 .976(6) . . ? C121 C122 1.385(7) . . ? C121 C126 1.383(6) . . ? C122 C123 1.401(6) . . ? C122 H122 .971(5) . . ? C123 C124 1.334(9) . . ? C123 H123 .961(6) . . ? C124 C125 1.357(9) . . ? C124 H124 .968(5) . . ? C125 C126 1.393(7) . . ? C125 H125 .965(5) . . ? C126 H126 .969(5) . . ? C0 P2 1.842(4) . . ? C0 H0a .960(4) . . ? C0 H0b .949(4) . . ? P2 C211 1.835(4) . . ? P2 C221 1.831(4) . . ? C211 C212 1.382(7) . . ? C211 C216 1.362(6) . . ? C212 C213 1.367(8) . . ? C212 H212 .964(5) . . ? C213 C214 1.350(8) . . ? C213 H213 .980(7) . . ? C214 C215 1.357(9) . . ? C214 H214 .967(5) . . ? C215 C216 1.380(7) . . ? C215 H215 .968(6) . . ? C216 H216 .972(6) . . ? C221 C222 1.387(7) . . ? C221 C226 1.386(7) . . ? C222 C223 1.390(9) . . ? C222 H222 .979(5) . . ? C223 C224 1.375(10) . . ? C223 H223 .981(7) . . ? C224 C225 1.341(12) . . ? C224 H224 .962(7) . . ? C225 C226 1.402(9) . . ? C225 H225 .987(7) . . ? C226 H226 .977(6) . . ? C01 C02 1.356(9) . . ? C01 C05 1.347(8) . . ? C01 H01 .961(5) . . ? C02 C03 1.406(8) . . ? C02 H02 .975(5) . . ? C03 C04 1.422(10) . . ? C03 H03 .953(7) . . ? C04 C05 1.417(10) . . ? C04 H04 .970(6) . . ? C05 H05 .985(6) . . ? Cl11 C110 1.94(3) . . ? Cl11 Cl21 1.670(15) . . ? Cl11 Cl22 1.55(3) . . ? Cl12 C110 1.60(3) . . ? Cl12 Cl22 1.56(3) . . ? Cl12 C210 1.20(4) . . ? Cl12 H210a 1.057(15) . . ? C110 Cl22 .99(3) . . ? C110 H110a 1.047(13) . . ? C110 H110b .940(15) . . ? Cl21 C210 1.89(4) . . ? Cl22 C210 1.54(4) . . ? Cl22 H110a 1.35(3) . . ? C210 H210a .82(3) . . ? C210 H210b 1.03(3) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W1 Co2 3.8386(6) . . ? W1 Co3 3.9591(7) . . ? W1 O11 3.131(4) . . ? W1 O12 3.120(5) . . ? W1 O13 3.122(4) . . ? W1 C22 3.850(5) . . ? W1 C2 3.399(4) . . ? W1 Cl21 4.678(11) . . ? W1 H01 3.0036(4) . . ? W1 H02 2.9470(3) . . ? W1 H03 2.9153(3) . . ? W1 H04 2.9118(4) . . ? W1 H05 2.9774(3) . . ? Co2 C13 3.604(5) . . ? Co2 O21 2.911(3) . . ? Co2 O22 2.908(4) . . ? Co2 C31 3.385(4) . . ? Co2 C3 3.160(4) . . ? Co2 C111 3.510(5) . . ? Co2 C112 3.712(6) . . ? Co2 C121 3.440(4) . . ? Co2 C126 3.762(5) . . ? Co2 C0 3.294(4) . . ? Co2 P2 3.3491(11) . . ? Co2 C01 3.727(5) . . ? Co2 H112 3.1559(6) . . ? Co2 H126 3.3757(6) . . ? Co2 H01 3.2126(6) . . ? Co3 C12 3.623(6) . . ? Co3 C21 2.945(5) . . ? Co3 O21 3.714(4) . . ? Co3 O31 2.924(3) . . ? Co3 O32 2.915(4) . . ? Co3 C3 3.022(3) . . ? Co3 P1 3.6270(12) . . ? Co3 C0 3.359(4) . . ? Co3 C211 3.531(4) . . ? Co3 C216 3.747(5) . . ? Co3 C221 3.487(4) . . ? Co3 H215 3.4563(6) . 2_655 ? Co3 H216 3.2101(6) . . ? C11 C12 2.480(7) . . ? C11 C13 2.467(8) . . ? C11 C04 2.970(8) . . ? C11 Cl21 3.509(11) . . ? O11 Cl21 3.212(9) . . ? O11 Cl22 3.88(3) . . ? O11 H210b 2.510(5) . . ? C12 C1 2.573(8) . . ? O12 Cl12 3.637(12) . 3_666 ? O12 H123 2.594(5) . 7_666 ? C13 C1 2.518(6) . . ? C13 Cl21 3.793(13) . . ? O13 Cl21 3.702(13) . . ? O13 H04 2.546(4) . 7_656 ? C21 C22 2.692(5) . . ? C21 C31 2.941(7) . . ? C21 P1 3.152(4) . . ? C21 P2 3.630(5) . . ? C21 H112 2.606(5) . . ? C21 H01 2.636(5) . . ? C22 C1 2.880(6) . . ? C22 P1 3.153(4) . . ? C22 H126 2.601(4) . . ? O22 H214 2.659(4) . 6_645 ? C31 C32 2.687(6) . . ? C31 C1 2.953(5) . . ? C31 P2 3.355(4) . . ? C31 Cl12 3.930(13) . 3_666 ? C31 H216 2.562(4) . . ? O31 O31 2.996(5) . 2_655 ? O31 Cl12 3.629(14) . 3_666 ? C32 C2 2.902(6) . . ? C32 P2 3.019(5) . . ? C32 Cl12 3.920(9) . 3_666 ? O32 P2 3.862(4) . . ? O32 Cl12 3.697(9) . 3_666 ? C1 C3 2.612(5) . . ? C1 P1 3.854(4) . . ? C1 P2 3.947(4) . . ? C2 C4 2.603(5) . . ? C2 P1 3.023(4) . . ? C2 P2 3.247(4) . . ? C3 C4 2.586(5) . 7_666 ? C3 P1 3.438(4) . . ? C3 P2 3.722(4) . . ? P1 C112 2.791(6) . . ? P1 C116 2.823(6) . . ? P1 C122 2.855(5) . . ? P1 C126 2.777(5) . . ? P1 P2 3.0176(14) . . ? P1 C211 3.725(4) . . ? P1 H112 2.8612(11) . . ? P1 H116 2.9285(11) . . ? P1 H122 2.9605(10) . . ? P1 H126 2.8271(10) . . ? P1 H0a 2.3317(10) . . ? P1 H0b 2.3317(11) . . ? C111 C113 2.409(8) . . ? C111 C114 2.782(8) . . ? C111 C115 2.413(8) . . ? C111 C121 2.873(6) . . ? C111 C0 2.900(6) . . ? C111 P2 3.965(4) . . ? C111 H112 2.031(4) . . ? C111 H116 2.052(4) . . ? C112 C114 2.370(9) . . ? C112 C115 2.731(9) . . ? C112 C116 2.362(7) . . ? C112 H113 2.066(6) . . ? C113 C115 2.350(10) . . ? C113 C116 2.742(9) . . ? C113 H112 2.051(7) . . ? C113 H114 2.019(7) . . ? C114 C116 2.393(9) . . ? C114 H113 1.991(8) . . ? C114 H115 2.050(8) . . ? C115 H114 2.011(7) . . ? C115 H116 2.065(7) . . ? C116 Cl12 3.719(11) . 7_666 ? C116 H115 2.057(6) . . ? C121 C123 2.418(7) . . ? C121 C124 2.777(6) . . ? C121 C125 2.422(6) . . ? C121 C0 2.882(5) . . ? C121 H122 2.037(4) . . ? C121 H126 2.032(4) . . ? C122 C124 2.373(7) . . ? C122 C125 2.746(7) . . ? C122 C126 2.363(7) . . ? C122 H123 2.053(5) . . ? C123 C125 2.344(9) . . ? C123 C126 2.728(8) . . ? C123 H122 2.075(5) . . ? C123 H124 1.996(5) . . ? C124 C126 2.371(7) . . ? C124 H123 1.996(7) . . ? C124 H125 2.024(7) . . ? C125 H124 2.016(6) . . ? C125 H126 2.055(5) . . ? C126 H125 2.057(4) . . ? C0 C211 2.908(5) . . ? C0 C221 2.834(6) . . ? C0 Cl11 3.874(7) . 7_666 ? C0 Cl21 3.761(8) . 7_666 ? C0 H122 2.650(3) . . ? P2 C212 2.833(6) . . ? P2 C216 2.764(4) . . ? P2 C222 2.782(6) . . ? P2 C226 2.828(5) . . ? P2 Cl11 4.585(6) . 7_666 ? P2 Cl21 4.878(8) . 7_666 ? P2 H0a 2.3357(10) . . ? P2 H0b 2.3353(9) . . ? P2 H212 2.9232(11) . . ? P2 H216 2.8385(9) . . ? P2 H222 2.8531(11) . . ? P2 H226 2.9277(10) . . ? C211 C213 2.386(8) . . ? C211 C214 2.763(7) . . ? C211 C215 2.384(6) . . ? C211 C221 2.852(6) . . ? C211 H212 2.028(4) . . ? C211 H216 2.028(4) . . ? C211 H226 2.557(4) . . ? C212 C214 2.365(7) . . ? C212 C215 2.719(7) . . ? C212 C216 2.353(8) . . ? C212 H213 2.040(5) . . ? C213 C215 2.336(9) . . ? C213 C216 2.716(9) . . ? C213 H212 2.038(5) . . ? C213 H214 2.026(5) . . ? C214 C216 2.375(8) . . ? C214 Cl22 3.69(3) . 4_564 ? C214 H213 2.017(6) . . ? C214 H215 2.019(6) . . ? C215 Cl12 3.755(13) . 4_564 ? C215 Cl22 3.64(3) . 4_564 ? C215 H214 2.019(6) . . ? C215 H216 2.042(6) . . ? C216 H215 2.044(4) . . ? C221 C223 2.408(9) . . ? C221 C224 2.783(8) . . ? C221 C225 2.413(8) . . ? C221 Cl11 3.704(8) . 7_666 ? C221 H222 2.052(4) . . ? C221 H226 2.048(4) . . ? C222 C224 2.398(8) . . ? C222 C225 2.747(8) . . ? C222 C226 2.384(8) . . ? C222 Cl11 3.660(10) . 7_666 ? C222 Cl21 3.700(10) . 7_666 ? C222 H223 2.066(6) . . ? C223 C225 2.352(10) . . ? C223 C226 2.750(10) . . ? C223 Cl11 3.782(13) . 7_666 ? C223 Cl21 3.915(12) . 7_666 ? C223 H222 2.066(7) . . ? C223 H224 2.040(7) . . ? C224 C226 2.387(10) . . ? C224 Cl11 3.939(12) . 7_666 ? C224 H223 2.044(8) . . ? C224 H225 2.035(8) . . ? C225 H224 1.998(8) . . ? C225 H226 2.080(8) . . ? C226 Cl11 3.866(9) . 7_666 ? C226 H225 2.059(5) . . ? C01 C03 2.249(9) . . ? C01 C04 2.242(7) . . ? C01 H02 2.090(7) . . ? C01 H05 2.085(6) . . ? C02 C04 2.259(8) . . ? C02 C05 2.214(8) . . ? C02 H01 2.058(6) . . ? C02 H03 2.129(6) . . ? C03 C05 2.276(10) . . ? C03 H02 2.115(6) . . ? C03 H04 2.153(6) . . ? C04 Cl11 3.890(11) . 7_656 ? C04 H03 2.128(9) . . ? C04 H05 2.144(8) . . ? C05 Cl11 3.834(9) . 7_656 ? C05 H01 2.059(6) . . ? C05 H04 2.138(7) . . ? Cl11 Cl12 2.837(12) . . ? Cl11 C210 2.43(3) . . ? Cl11 H113 3.339(10) . 4_565 ? Cl11 H0a 3.224(6) . 7_666 ? Cl11 H212 3.588(10) . 7_666 ? Cl11 H05 3.540(6) . 7_656 ? Cl11 H110a 2.313(12) . . ? Cl11 H110b 2.327(12) . . ? Cl11 H210a 2.907(7) . . ? Cl11 H210b 3.099(8) . . ? Cl12 Cl21 2.819(18) . . ? Cl12 H116 2.800(8) . 7_666 ? Cl12 H122 3.421(12) . 7_666 ? Cl12 H0a 3.544(8) . 7_666 ? Cl12 H215 3.191(11) . 4_565 ? Cl12 H02 3.511(9) . 3_666 ? Cl12 H110a 2.292(10) . . ? Cl12 H110b 2.280(10) . . ? Cl12 H210b 2.047(14) . . ? C110 Cl21 2.85(2) . . ? C110 C210 2.14(3) . . ? C110 H210a 2.320(18) . . ? Cl21 Cl22 2.25(4) . . ? Cl21 H122 3.046(7) . 7_666 ? Cl21 H0a 3.354(9) . 7_666 ? Cl21 H0b 3.251(7) . 7_666 ? Cl21 H04 3.523(9) . 7_656 ? Cl21 H110a 3.506(12) . . ? Cl21 H110b 3.364(12) . . ? Cl21 H210a 2.275(11) . . ? Cl21 H210b 2.265(9) . . ? Cl22 H0a 3.60(2) . 7_666 ? Cl22 H214 3.56(2) . 4_565 ? Cl22 H215 3.45(3) . 4_565 ? Cl22 H110b 1.88(3) . . ? Cl22 H210a 2.05(3) . . ? Cl22 H210b 2.31(3) . . ? H112 H113 2.3804(2) . . ? H113 H114 2.2966(3) . . ? H114 H115 2.3322(2) . . ? H115 H116 2.3556(2) . . ? H116 H0a 2.3631(2) . . ? H122 H123 2.3749(2) . . ? H122 H0b 2.1794(2) . . ? H123 H124 2.2905(2) . . ? H124 H125 2.3197(2) . . ? H125 H126 2.3653(2) . . ? H0a H0b 1.55141(18) . . ? H0a H212 2.1165(2) . . ? H212 H213 2.3520(3) . . ? H212 H110b 2.1151(2) . 7_666 ? H213 H214 2.32595(16) . . ? H214 H215 2.31404(18) . . ? H215 H216 2.3433(3) . . ? H222 H223 2.3805(2) . . ? H223 H224 2.34589(19) . . ? H224 H225 2.3237(3) . . ? H225 H226 2.3676(2) . . ? H110a H110b 1.5513(2) . . ? H210a H210b 1.55115(17) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 W1 C12 78.2(2) . . . ? C11 W1 C13 76.7(2) . . . ? C11 W1 C1 132.79(18) . . . ? C11 W1 C01 143.9(2) . . . ? C11 W1 C02 123.2(2) . . . ? C11 W1 C03 90.2(2) . . . ? C11 W1 C04 87.4(2) . . . ? C11 W1 C05 118.4(2) . . . ? C12 W1 C13 105.7(2) . . . ? C12 W1 C1 76.0(2) . . . ? C12 W1 C01 121.5(2) . . . ? C12 W1 C02 97.2(2) . . . ? C12 W1 C03 103.5(2) . . . ? C12 W1 C04 137.2(3) . . . ? C12 W1 C05 153.1(2) . . . ? C13 W1 C1 73.28(16) . . . ? C13 W1 C01 119.5(2) . . . ? C13 W1 C02 152.8(2) . . . ? C13 W1 C03 144.6(2) . . . ? C13 W1 C04 109.8(2) . . . ? C13 W1 C05 99.1(2) . . . ? C1 W1 C01 83.17(15) . . . ? C1 W1 C02 98.84(16) . . . ? C1 W1 C03 133.95(17) . . . ? C1 W1 C04 136.9(2) . . . ? C1 W1 C05 101.81(19) . . . ? C01 W1 C02 33.4(2) . . . ? C01 W1 C03 57.4(2) . . . ? C01 W1 C04 57.3(2) . . . ? C01 W1 C05 33.16(19) . . . ? C02 W1 C03 35.1(2) . . . ? C02 W1 C04 58.1(2) . . . ? C02 W1 C05 56.3(2) . . . ? C03 W1 C04 35.8(3) . . . ? C03 W1 C05 58.4(2) . . . ? C04 W1 C05 35.4(3) . . . ? Co3 Co2 C21 87.03(15) . . . ? Co3 Co2 C22 151.33(16) . . . ? Co3 Co2 C1 52.72(10) . . . ? Co3 Co2 C2 51.78(9) . . . ? Co3 Co2 P1 101.48(4) . . . ? C21 Co2 C22 99.6(2) . . . ? C21 Co2 C1 112.31(18) . . . ? C21 Co2 C2 138.19(18) . . . ? C21 Co2 P1 104.42(16) . . . ? C22 Co2 C1 99.5(2) . . . ? C22 Co2 C2 113.52(18) . . . ? C22 Co2 P1 103.74(15) . . . ? C1 Co2 C2 39.89(15) . . . ? C1 Co2 P1 132.03(11) . . . ? C2 Co2 P1 92.17(11) . . . ? Co2 Co3 C31 104.59(15) . . . ? Co2 Co3 C32 151.97(13) . . . ? Co2 Co3 C1 51.80(12) . . . ? Co2 Co3 C2 51.24(12) . . . ? Co2 Co3 P2 90.67(4) . . . ? C31 Co3 C32 97.7(2) . . . ? C31 Co3 C1 101.47(16) . . . ? C31 Co3 C2 140.43(17) . . . ? C31 Co3 P2 112.12(14) . . . ? C32 Co3 C1 107.50(18) . . . ? C32 Co3 C2 100.75(17) . . . ? C32 Co3 P2 96.51(16) . . . ? C1 Co3 C2 39.47(14) . . . ? C1 Co3 P2 135.35(11) . . . ? C2 Co3 P2 100.19(11) . . . ? W1 C11 O11 179.5(5) . . . ? W1 C12 O12 176.5(5) . . . ? W1 C13 O13 179.4(4) . . . ? Co2 C21 O21 178.1(4) . . . ? Co2 C22 O22 177.4(4) . . . ? Co3 C31 O31 174.0(4) . . . ? Co3 C32 O32 177.0(4) . . . ? W1 C1 Co2 131.5(2) . . . ? W1 C1 Co3 138.38(18) . . . ? W1 C1 C2 143.7(3) . . . ? Co2 C1 Co3 75.48(13) . . . ? Co2 C1 C2 68.9(2) . . . ? Co3 C1 C2 68.7(2) . . . ? Co2 C2 Co3 76.98(12) . . . ? Co2 C2 C1 71.2(2) . . . ? Co2 C2 C3 139.0(3) . . . ? Co3 C2 C1 71.8(2) . . . ? Co3 C2 C3 125.9(3) . . . ? C1 C2 C3 143.5(4) . . . ? C2 C3 C4 170.9(4) . . . ? C3 C4 C4 179.3(4) . . 7_666 ? Co2 P1 C111 119.70(14) . . . ? Co2 P1 C121 115.61(14) . . . ? Co2 P1 C0 108.45(14) . . . ? C111 P1 C121 103.10(19) . . . ? C111 P1 C0 104.7(2) . . . ? C121 P1 C0 103.63(18) . . . ? P1 C111 C112 120.2(4) . . . ? P1 C111 C116 122.1(4) . . . ? C112 C111 C116 117.7(5) . . . ? C111 C112 C113 121.4(5) . . . ? C111 C112 H112 118.7(5) . . . ? C113 C112 H112 119.9(5) . . . ? C112 C113 C114 120.3(6) . . . ? C112 C113 H113 121.9(7) . . . ? C114 C113 H113 117.9(7) . . . ? C113 C114 C115 120.1(6) . . . ? C113 C114 H114 121.2(8) . . . ? C115 C114 H114 118.7(8) . . . ? C114 C115 C116 120.1(6) . . . ? C114 C115 H115 121.1(7) . . . ? C116 C115 H115 118.8(6) . . . ? C111 C116 C115 120.4(5) . . . ? C111 C116 H116 119.8(6) . . . ? C115 C116 H116 119.8(6) . . . ? P1 C121 C122 124.2(3) . . . ? P1 C121 C126 118.5(3) . . . ? C122 C121 C126 117.2(4) . . . ? C121 C122 C123 120.4(5) . . . ? C121 C122 H122 118.6(4) . . . ? C123 C122 H122 120.9(5) . . . ? C122 C123 C124 120.4(5) . . . ? C122 C123 H123 119.6(5) . . . ? C124 C123 H123 120.0(5) . . . ? C123 C124 C125 121.2(5) . . . ? C123 C124 H124 119.4(7) . . . ? C125 C124 H124 119.4(6) . . . ? C124 C125 C126 119.2(5) . . . ? C124 C125 H125 120.4(5) . . . ? C126 C125 H125 120.5(5) . . . ? C121 C126 C125 121.6(4) . . . ? C121 C126 H126 118.5(4) . . . ? C125 C126 H126 119.9(5) . . . ? P1 C0 P2 110.5(2) . . . ? P1 C0 H0a 109.4(3) . . . ? P1 C0 H0b 110.0(3) . . . ? P2 C0 H0a 108.8(3) . . . ? P2 C0 H0b 109.4(3) . . . ? H0a C0 H0b 108.7(4) . . . ? Co3 P2 C0 110.19(13) . . . ? Co3 P2 C211 119.53(13) . . . ? Co3 P2 C221 117.27(16) . . . ? C0 P2 C211 104.5(2) . . . ? C0 P2 C221 101.00(18) . . . ? C211 P2 C221 102.1(2) . . . ? P2 C211 C212 122.8(3) . . . ? P2 C211 C216 118.9(4) . . . ? C212 C211 C216 118.1(4) . . . ? C211 C212 C213 120.5(5) . . . ? C211 C212 H212 118.6(5) . . . ? C213 C212 H212 121.0(6) . . . ? C212 C213 C214 121.0(6) . . . ? C212 C213 H213 119.9(5) . . . ? C214 C213 H213 119.1(6) . . . ? C213 C214 C215 119.3(5) . . . ? C213 C214 H214 121.0(6) . . . ? C215 C214 H214 119.7(5) . . . ? C214 C215 C216 120.4(5) . . . ? C214 C215 H215 119.6(5) . . . ? C216 C215 H215 120.0(6) . . . ? C211 C216 C215 120.7(5) . . . ? C211 C216 H216 119.7(4) . . . ? C215 C216 H216 119.5(5) . . . ? P2 C221 C222 119.0(3) . . . ? P2 C221 C226 122.5(4) . . . ? C222 C221 C226 118.6(5) . . . ? C221 C222 C223 120.3(5) . . . ? C221 C222 H222 119.3(5) . . . ? C223 C222 H222 120.4(6) . . . ? C222 C223 C224 120.3(7) . . . ? C222 C223 H223 120.2(6) . . . ? C224 C223 H223 119.4(7) . . . ? C223 C224 C225 120.0(7) . . . ? C223 C224 H224 120.5(8) . . . ? C225 C224 H224 119.4(7) . . . ? C224 C225 C226 120.9(6) . . . ? C224 C225 H225 121.1(7) . . . ? C226 C225 H225 118.0(7) . . . ? C221 C226 C225 119.9(6) . . . ? C221 C226 H226 119.2(5) . . . ? C225 C226 H226 120.9(6) . . . ? W1 C01 C02 72.3(3) . . . ? W1 C01 C05 72.7(3) . . . ? W1 C01 H01 123.1(4) . . . ? C02 C01 C05 110.0(5) . . . ? C02 C01 H01 124.5(5) . . . ? C05 C01 H01 125.5(7) . . . ? W1 C02 C01 74.2(3) . . . ? W1 C02 C03 71.2(3) . . . ? W1 C02 H02 119.3(4) . . . ? C01 C02 C03 109.0(5) . . . ? C01 C02 H02 126.6(5) . . . ? C03 C02 H02 124.3(6) . . . ? W1 C03 C02 73.6(3) . . . ? W1 C03 C04 71.8(3) . . . ? W1 C03 H03 120.4(5) . . . ? C02 C03 C04 106.0(6) . . . ? C02 C03 H03 127.9(6) . . . ? C04 C03 H03 126.1(6) . . . ? W1 C04 C03 72.3(3) . . . ? W1 C04 C05 74.0(3) . . . ? W1 C04 H04 119.6(4) . . . ? C03 C04 C05 106.5(5) . . . ? C03 C04 H04 127.3(8) . . . ? C05 C04 H04 126.1(8) . . . ? W1 C05 C01 74.2(4) . . . ? W1 C05 C04 70.6(4) . . . ? W1 C05 H05 120.8(4) . . . ? C01 C05 C04 108.4(6) . . . ? C01 C05 H05 126.2(7) . . . ? C04 C05 H05 125.4(6) . . . ? C110 Cl11 Cl21 103.9(8) . . . ? C110 Cl11 Cl22 30.5(12) . . . ? Cl21 Cl11 Cl22 88.6(13) . . . ? C110 Cl12 Cl22 36.7(13) . . . ? C110 Cl12 C210 98.7(17) . . . ? C110 Cl12 H210a 120.6(12) . . . ? Cl22 Cl12 C210 66(2) . . . ? Cl22 Cl12 H210a 101.3(16) . . . ? C210 Cl12 H210a 41.8(15) . . . ? Cl11 C110 Cl12 106.0(10) . . . ? Cl11 C110 Cl22 52(2) . . . ? Cl11 C110 H110a 96.6(18) . . . ? Cl11 C110 H110b 102(2) . . . ? Cl12 C110 Cl22 69(2) . . . ? Cl12 C110 H110a 119(2) . . . ? Cl12 C110 H110b 126.0(19) . . . ? Cl22 C110 H110a 83.0(19) . . . ? Cl22 C110 H110b 154(4) . . . ? H110a C110 H110b 102.5(13) . . . ? Cl11 Cl21 C210 85.9(11) . . . ? Cl11 Cl22 Cl12 132.0(19) . . . ? Cl11 Cl22 C110 97(3) . . . ? Cl11 Cl22 C210 104(2) . . . ? Cl11 Cl22 H110a 105.5(18) . . . ? Cl12 Cl22 C110 74(2) . . . ? Cl12 Cl22 C210 45.8(16) . . . ? Cl12 Cl22 H110a 104(2) . . . ? C110 Cl22 C210 114(3) . . . ? C110 Cl22 H110a 50.2(17) . . . ? C210 Cl22 H110a 148(3) . . . ? Cl12 C210 Cl21 130(2) . . . ? Cl12 C210 Cl22 68(2) . . . ? Cl12 C210 H210a 59(2) . . . ? Cl12 C210 H210b 132(3) . . . ? Cl21 C210 Cl22 81(2) . . . ? Cl21 C210 H210a 108(3) . . . ? Cl21 C210 H210b 97(2) . . . ? Cl22 C210 H210a 117(3) . . . ? Cl22 C210 H210b 127(3) . . . ? H210a C210 H210b 113(3) . . . ? C110 H110a Cl22 46.8(13) . . . ? Cl12 H210a C210 79(2) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_author ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 _publ_contact_author_fax (61)-8-9380-1005 _publ_contact_author_email bws@crystal.uwa.edu.au loop_ _publ_author_name _publ_author_address '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=END data_br599 _audit_creation_date 98-08-31 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common 'compound 6' _chemical_formula_analytical C94_H66_Co4_O14_P4_W2 _chemical_formula_moiety ? _chemical_formula_structural C82_H54_Co4_O14_P4_W2.2C6_H6 _chemical_formula_sum C94_H66_Co4_O14_P4_W2 _chemical_formula_weight 2146.88 _chemical_melting_point ? _computing_data_collection 'Bruker SMART software' _computing_cell_refinement 'Bruker SAINT software' _computing_data_reduction 'Bruker SAINT software' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 18.3040(10) _cell_length_b 14.0866(8) _cell_length_c 18.7290(10) _cell_angle_alpha 90.00000 _cell_angle_beta 115.7390(10) _cell_angle_gamma 90.00000 _cell_volume 4350.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 0 _cell_measurement_theta_max 29 _cell_special_details ; ? ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _exptl_crystal_description block _exptl_crystal_preparation ? _exptl_crystal_colour dark _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2116 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_absorpt_coefficient_mu 3.52 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.77 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 300 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device 'Bruker area detector diffractometer' _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 44160 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI .139 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 29.13 _diffrn_reflns_reduction_process ? loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 188 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 132 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Co ? 0 8 .299 .973 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 28 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 8 .09 .095 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 W ? 0 4 -1.421 6.872 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom W1 .601044(16) .52066(2) .359215(13) .05977(15) Uani ? ? Co2 .62057(4) .39274(5) .04200(4) .0397(3) Uani ? ? Co3 .64162(4) .56708(5) .05116(4) .0420(4) Uani ? ? C11 .6716(5) .6008(7) .4504(4) .104(6) Uani ? ? O11 .7121(4) .6493(6) .5015(3) .167(6) Uani ? ? C12 .7059(5) .4647(6) .3860(4) .091(5) Uani ? ? O12 .7677(4) .4273(5) .4022(3) .129(5) Uani ? ? C13 .5923(5) .6475(6) .3079(4) .088(5) Uani ? ? O13 .5844(5) .7197(4) .2779(4) .140(5) Uani ? ? C21 .5732(3) .2948(5) .0615(4) .064(4) Uani ? ? O21 .5438(3) .2333(4) .0791(3) .115(4) Uani ? ? C22 .6058(3) .3744(5) -.0573(4) .067(4) Uani ? ? O22 .5926(3) .3665(5) -.1228(3) .116(4) Uani ? ? C31 .6139(3) .6794(5) .0722(4) .070(4) Uani ? ? O31 .5951(3) .7514(4) .0886(4) .117(4) Uani ? ? C32 .6443(3) .5881(5) -.0416(4) .071(4) Uani ? ? O32 .6448(3) .6009(5) -.1012(3) .136(5) Uani ? ? C1 .5997(3) .4972(4) .2467(3) .050(3) Uani ? ? C2 .5946(3) .4902(4) .1798(3) .045(3) Uani ? ? C3 .5929(3) .4867(4) .1046(3) .037(2) Uani ? ? C4 .5417(3) .4936(3) .0263(3) .036(2) Uani ? ? P1 .74531(8) .35536(11) .12939(7) .0440(7) Uani ? ? C111 .7501(3) .2529(5) .1906(3) .059(3) Uani ? ? C112 .7245(6) .2591(6) .2494(4) .111(6) Uani ? ? C113 .7212(7) .1813(9) .2914(5) .142(8) Uani ? ? C114 .7419(6) .0972(10) .2760(8) .153(9) Uani ? ? C115 .7632(7) .0878(8) .2151(10) .207(11) Uani ? ? C116 .7674(6) .1660(6) .1728(7) .130(7) Uani ? ? C121 .8272(3) .3283(4) .1010(3) .050(3) Uani ? ? C122 .8102(4) .3094(6) .0244(4) .078(4) Uani ? ? C123 .8726(4) .2867(7) .0028(4) .103(6) Uani ? ? C124 .9508(4) .2822(6) .0600(5) .083(5) Uani ? ? C125 .9675(4) .3001(6) .1348(4) .083(4) Uani ? ? C126 .9063(3) .3224(6) .1567(3) .075(4) Uani ? ? C0 .7847(3) .4516(4) .2010(3) .044(3) Uani ? ? P2 .76761(8) .56505(11) .14812(7) .0453(7) Uani ? ? C211 .7891(3) .6516(5) .2269(3) .054(3) Uani ? ? C212 .7999(4) .6312(6) .3019(4) .094(5) Uani ? ? C213 .8102(6) .7027(9) .3565(5) .124(7) Uani ? ? C214 .8090(6) .7924(9) .3370(7) .121(7) Uani ? ? C215 .8015(6) .8165(6) .2659(7) .123(6) Uani ? ? C216 .7891(4) .7442(6) .2076(4) .089(5) Uani ? ? C221 .8579(3) .5744(4) .1303(3) .054(3) Uani ? ? C222 .9337(3) .5859(6) .1928(4) .084(5) Uani ? ? C223 1.0026(4) .5885(7) .1780(5) .105(6) Uani ? ? C224 .9971(5) .5783(7) .1059(6) .103(6) Uani ? ? C225 .9242(5) .5652(7) .0438(5) .107(6) Uani ? ? C226 .8534(4) .5652(6) .0558(4) .082(4) Uani ? ? C01 .4785(7) .4360(11) .3013(6) .117(8) Uani ? ? C02 .5354(7) .3809(6) .3629(8) .123(7) Uani ? ? C03 .5534(6) .4321(9) .4332(5) .115(7) Uani ? ? C04 .5112(8) .5158(8) .4136(7) .118(7) Uani ? ? C05 .4662(6) .5175(9) .3344(10) .136(9) Uani ? ? C101 .9176(9) 1.0098(11) .0993(8) .136(9) Uani ? ? C102 .8967(8) .9342(17) .1160(9) .162(12) Uani ? ? C103 .9354(11) .8485(13) .1185(8) .164(12) Uani ? ? C104 1.0047(11) .8457(10) .1098(7) .126(9) Uani ? ? C105 1.0311(7) .9169(18) .0982(6) .141(10) Uani ? ? C106 .9920(14) 1.0088(11) .0888(7) .174(12) Uani ? ? H112 .70859 .32108 .26228 .13600 Uiso ? ? H113 .70621 .18215 .33475 .16600 Uiso ? ? H114 .74201 .03838 .30384 .17500 Uiso ? ? H115 .77557 .02299 .19930 .21600 Uiso ? ? H116 .78460 .15993 .13060 .15700 Uiso ? ? H122 .75472 .31084 -.01589 .09700 Uiso ? ? H123 .86176 .27261 -.05135 .12700 Uiso ? ? H124 .99395 .26656 .04493 .10100 Uiso ? ? H125 1.02385 .29682 .17598 .10400 Uiso ? ? H126 .92024 .33633 .21268 .09600 Uiso ? ? H0a .84131 .44318 .23365 .05600 Uiso ? ? H0b .75737 .45248 .23486 .05600 Uiso ? ? H212 .80025 .56493 .31814 .12000 Uiso ? ? H213 .81897 .69123 .41017 .14500 Uiso ? ? H214 .81255 .84619 .37135 .14400 Uiso ? ? H215 .80102 .88519 .24680 .15300 Uiso ? ? H216 .78212 .76153 .15369 .10900 Uiso ? ? H222 .93853 .59305 .24643 .10400 Uiso ? ? H223 1.05648 .59640 .22412 .12300 Uiso ? ? H224 1.04605 .57986 .09827 .13000 Uiso ? ? H225 .92052 .55815 -.00912 .12900 Uiso ? ? H226 .80061 .55644 .01070 .10100 Uiso ? ? H01 .45047 .42354 .24656 .14900 Uiso ? ? H02 .55787 .32036 .35680 .14900 Uiso ? ? H03 .59244 .41281 .48678 .14000 Uiso ? ? H04 .51599 .56460 .45296 .15200 Uiso ? ? H05 .43200 .57366 .30902 .15300 Uiso ? ? H101 .88593 1.06862 .09127 .17100 Uiso ? ? H102 .85236 .93365 .13059 .19400 Uiso ? ? H103 .91463 .78822 .12281 .19400 Uiso ? ? H104 1.03914 .78996 .11450 .15100 Uiso ? ? H105 1.08317 .92063 .09290 .17500 Uiso ? ? H106 1.01394 1.06956 .07931 .20500 Uiso ? ? 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 W1 .08126(19) .06703(19) .04204(12) .01135(15) .03709(12) .00248(13) Co2 .0359(4) .0470(5) .0364(3) .0052(3) .0160(3) -.0017(3) Co3 .0369(4) .0491(5) .0385(3) -.0001(3) .0148(3) .0041(3) C11 .116(6) .120(8) .066(5) .022(5) .032(4) -.021(5) O11 .179(7) .200(8) .084(4) .001(6) .021(4) -.067(5) C12 .118(7) .109(7) .046(4) .038(5) .036(4) .005(4) O12 .114(5) .173(7) .089(4) .055(5) .036(3) .011(4) C13 .132(7) .071(6) .060(4) .011(5) .039(4) -.004(4) O13 .222(7) .066(4) .120(5) .001(5) .062(5) .015(4) C21 .047(4) .061(5) .072(4) .007(3) .015(3) .007(3) O21 .084(4) .083(4) .155(5) -.020(3) .031(3) .043(4) C22 .064(4) .078(5) .058(4) .022(3) .025(3) -.006(3) O22 .134(4) .167(6) .047(3) .043(4) .040(3) -.017(3) C31 .040(3) .062(5) .088(5) .003(3) .008(3) .005(4) O31 .085(4) .068(4) .167(5) .016(3) .026(4) -.027(4) C32 .055(4) .095(6) .055(4) -.019(3) .016(3) .011(4) O32 .132(5) .223(8) .054(3) -.039(5) .042(3) .035(4) C1 .044(3) .052(4) .052(3) .003(2) .020(2) -.005(3) C2 .036(3) .061(4) .039(2) .006(2) .018(2) .004(2) C3 .027(2) .045(3) .038(2) .002(2) .014(2) -.000(2) C4 .035(2) .039(3) .037(2) .005(2) .019(2) .001(2) P1 .0376(7) .0546(10) .0412(7) .0092(6) .0184(6) .0067(7) C111 .039(3) .064(5) .066(4) .009(3) .016(3) .020(3) C112 .188(9) .089(7) .078(5) -.047(6) .078(6) -.004(4) C113 .190(11) .152(11) .073(5) -.068(9) .046(6) .028(7) C114 .079(6) .154(11) .202(12) .006(7) .040(7) .137(11) C115 .173(10) .088(8) .46(2) .070(7) .225(14) .130(12) C116 .155(8) .072(7) .242(11) .051(6) .159(8) .067(7) C121 .045(3) .052(4) .059(3) .009(3) .027(3) .005(3) C122 .051(4) .121(7) .063(4) .007(4) .025(3) -.013(4) C123 .070(5) .167(9) .088(5) .011(5) .050(4) -.035(5) C124 .060(4) .100(6) .107(6) .014(4) .053(4) -.006(5) C125 .042(4) .123(7) .082(5) .020(4) .025(3) .007(5) C126 .047(4) .119(6) .060(4) .021(4) .022(3) .006(4) C0 .042(3) .059(4) .030(2) .004(2) .013(2) .003(2) P2 .0379(7) .0573(10) .0398(7) -.0036(7) .0161(6) -.0032(7) C211 .040(3) .063(5) .058(3) -.004(3) .019(3) -.008(3) C212 .111(6) .110(7) .072(5) -.037(5) .051(4) -.034(4) C213 .151(8) .157(10) .096(6) -.063(8) .083(6) -.067(7) C214 .112(7) .136(10) .122(8) -.026(7) .058(6) -.083(8) C215 .124(8) .069(6) .141(9) .010(5) .026(7) -.020(7) C216 .094(5) .085(7) .074(5) -.003(4) .023(4) -.021(5) C221 .051(3) .064(4) .053(3) -.004(3) .028(3) -.003(3) C222 .043(4) .135(7) .076(4) -.010(4) .027(3) -.013(4) C223 .047(4) .144(8) .125(7) -.013(4) .038(4) -.015(6) C224 .069(5) .131(8) .133(8) .004(5) .066(6) .006(6) C225 .098(6) .163(9) .087(5) .022(6) .066(5) .021(6) C226 .062(4) .125(7) .064(4) .004(4) .031(3) .004(4) C01 .119(8) .159(11) .092(6) -.061(8) .062(6) -.012(7) C02 .176(10) .080(7) .187(11) -.022(7) .149(9) -.013(8) C03 .156(8) .125(9) .104(7) .017(7) .094(6) .043(6) C04 .159(9) .117(9) .137(9) .027(7) .119(8) .028(7) C05 .080(6) .144(11) .195(13) .017(7) .069(8) .053(10) C101 .121(10) .148(13) .135(9) .016(8) .050(8) .012(8) C102 .127(10) .185(17) .203(14) -.029(11) .101(9) -.016(14) C103 .161(13) .171(16) .182(12) -.062(11) .094(11) -.028(11) C104 .181(15) .090(9) .098(7) .000(8) .053(8) -.001(6) C105 .115(9) .211(17) .083(7) .019(12) .031(6) -.027(10) C106 .251(19) .142(13) .121(9) -.049(12) .072(11) .010(8) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 6205 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .093 _refine_ls_R_factor_obs .04 _refine_ls_wR_factor_all .048 _refine_ls_wR_factor_obs .041 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.199 _refine_ls_shift/esd_max .07 _refine_ls_shift/esd_mean .002 _refine_diff_density_min -.763 _refine_diff_density_max 1.751 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C11 1.986(8) . . ? W1 C12 1.929(9) . . ? W1 C13 2.002(8) . . ? W1 C1 2.123(6) . . ? W1 C01 2.349(12) . . ? W1 C02 2.323(11) . . ? W1 C03 2.299(12) . . ? W1 C04 2.280(16) . . ? W1 C05 2.305(12) . . ? Co2 Co3 2.4802(11) . . ? Co2 C21 1.750(7) . . ? Co2 C22 1.778(7) . . ? Co2 C3 1.975(5) . . ? Co2 C4 1.955(5) . . ? Co2 P1 2.2190(12) . . ? Co3 C31 1.758(8) . . ? Co3 C32 1.783(7) . . ? Co3 C3 1.964(6) . . ? Co3 C4 1.973(5) . . ? Co3 P2 2.2315(12) . . ? C11 O11 1.147(10) . . ? C12 O12 1.161(11) . . ? C13 O13 1.140(10) . . ? C21 O21 1.141(10) . . ? C22 O22 1.148(8) . . ? C31 O31 1.154(10) . . ? C32 O32 1.135(9) . . ? C1 C2 1.219(8) . . ? C2 C3 1.395(8) . . ? C3 C4 1.358(6) . . ? C4 C4 1.424(6) . 3_665 ? P1 C111 1.821(7) . . ? P1 C121 1.834(7) . . ? P1 C0 1.821(5) . . ? C111 C112 1.374(13) . . ? C111 C116 1.342(12) . . ? C112 C113 1.366(16) . . ? C112 H112 .983(9) . . ? C113 C114 1.31(2) . . ? C113 H113 .963(13) . . ? C114 C115 1.36(3) . . ? C114 H114 .978(14) . . ? C115 C116 1.379(18) . . ? C115 H115 1.015(13) . . ? C116 H116 .974(14) . . ? C121 C122 1.356(9) . . ? C121 C126 1.371(7) . . ? C122 C123 1.404(12) . . ? C122 H122 .968(5) . . ? C123 C124 1.367(9) . . ? C123 H123 .965(8) . . ? C124 C125 1.320(12) . . ? C124 H124 .974(9) . . ? C125 C126 1.387(11) . . ? C125 H125 .985(5) . . ? C126 H126 .984(6) . . ? C0 P2 1.834(5) . . ? C0 H0a .954(4) . . ? C0 H0b .963(6) . . ? P2 C211 1.821(7) . . ? P2 C221 1.827(7) . . ? C211 C212 1.360(10) . . ? C211 C216 1.354(11) . . ? C212 C213 1.389(14) . . ? C212 H212 .982(8) . . ? C213 C214 1.313(18) . . ? C213 H213 .960(10) . . ? C214 C215 1.321(18) . . ? C214 H214 .978(13) . . ? C215 C216 1.438(14) . . ? C215 H215 1.030(10) . . ? C216 H216 .991(8) . . ? C221 C222 1.382(7) . . ? C221 C226 1.368(10) . . ? C222 C223 1.406(12) . . ? C222 H222 .973(7) . . ? C223 C224 1.318(15) . . ? C223 H223 .996(6) . . ? C224 C225 1.349(10) . . ? C224 H224 .967(10) . . ? C225 C226 1.408(13) . . ? C225 H225 .969(9) . . ? C226 H226 .976(5) . . ? C01 C02 1.406(15) . . ? C01 C05 1.37(2) . . ? C01 H01 .942(9) . . ? C02 C03 1.408(18) . . ? C02 H02 .974(11) . . ? C03 C04 1.369(16) . . ? C03 H03 .985(8) . . ? C04 C05 1.35(2) . . ? C04 H04 .984(13) . . ? C05 H05 .992(12) . . ? C101 C102 1.22(3) . . ? C101 C106 1.46(3) . . ? C101 H101 .984(16) . . ? C102 C103 1.39(3) . . ? C102 H102 .961(18) . . ? C103 C104 1.35(3) . . ? C103 H103 .95(2) . . ? C104 C105 1.17(3) . . ? C104 H104 .987(16) . . ? C105 C106 1.45(3) . . ? C105 H105 1.001(14) . . ? C106 H106 .99(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W1 O11 3.133(6) . . ? W1 O12 3.090(7) . . ? W1 O13 3.141(6) . . ? W1 C2 3.339(6) . . ? W1 H01 2.9781(3) . . ? W1 H02 2.9252(3) . . ? W1 H03 2.8928(3) . . ? W1 H04 2.8746(3) . . ? W1 H05 2.9135(3) . . ? Co2 Co3 4.3730(9) . 3_665 ? Co2 O21 2.889(6) . . ? Co2 O22 2.924(5) . . ? Co2 C32 3.287(7) . . ? Co2 C2 3.136(6) . . ? Co2 C4 3.118(5) . 3_665 ? Co2 C111 3.393(5) . . ? Co2 C121 3.566(5) . . ? Co2 C0 3.288(4) . . ? Co2 P2 3.5270(15) . . ? Co2 H122 3.2938(8) . . ? Co2 H0b 3.4885(6) . . ? Co3 C22 3.281(7) . . ? Co3 O31 2.911(6) . . ? Co3 O32 2.918(6) . . ? Co3 C2 3.085(6) . . ? Co3 C4 3.141(4) . 3_665 ? Co3 P1 3.4969(16) . . ? Co3 C0 3.317(4) . . ? Co3 C211 3.439(5) . . ? Co3 C221 3.575(5) . . ? Co3 H226 3.3137(8) . . ? C11 C12 2.487(13) . . ? C11 C13 2.509(10) . . ? C11 C04 2.961(16) . . ? C12 C1 2.528(8) . . ? O12 H105 2.693(7) . 2_745 ? C13 C1 2.441(10) . . ? C21 C22 2.777(11) . . ? C21 C3 2.801(9) . . ? C21 C4 2.878(8) . . ? C21 P1 2.965(6) . . ? O21 P1 3.798(6) . . ? O21 H04 2.576(5) . 2_645 ? C22 C4 2.871(9) . . ? C22 P1 3.326(5) . . ? C22 H122 2.645(6) . . ? O22 H113 2.620(6) . 4_554 ? O22 H02 2.696(6) . 4_554 ? C31 C32 2.745(11) . . ? C31 C3 2.843(9) . . ? C31 C4 2.889(8) . . ? C31 P2 3.009(6) . . ? O31 P2 3.878(6) . . ? C32 C4 2.998(9) . . ? C32 P2 3.295(5) . . ? C32 H226 2.629(6) . . ? O32 H01 2.539(4) . 3_665 ? C1 C3 2.613(8) . . ? C1 C01 2.946(16) . . ? C2 C4 2.604(7) . . ? C2 P1 3.791(6) . . ? C2 P2 3.623(6) . . ? C3 C4 2.629(5) . 3_665 ? C3 P1 3.210(5) . . ? C3 P2 3.138(5) . . ? C4 P1 3.894(5) . . ? C4 P2 3.889(4) . . ? P1 C112 2.789(10) . . ? P1 C116 2.766(9) . . ? P1 C122 2.779(8) . . ? P1 C126 2.802(7) . . ? P1 P2 2.982(2) . . ? P1 C221 3.706(6) . . ? P1 H112 2.8867(16) . . ? P1 H116 2.8429(15) . . ? P1 H122 2.8694(16) . . ? P1 H126 2.9016(12) . . ? P1 H0a 2.3347(12) . . ? P1 H0b 2.3332(15) . . ? C111 C113 2.394(15) . . ? C111 C114 2.758(16) . . ? C111 C115 2.363(13) . . ? C111 C121 2.826(10) . . ? C111 C0 2.857(9) . . ? C111 H112 2.047(7) . . ? C111 H116 1.998(7) . . ? C112 C114 2.327(16) . . ? C112 C115 2.671(16) . . ? C112 C116 2.317(16) . . ? C112 H113 2.076(10) . . ? C113 C115 2.31(2) . . ? C113 C116 2.71(2) . . ? C113 H112 2.030(13) . . ? C113 H114 2.043(13) . . ? C114 C116 2.38(2) . . ? C114 H113 1.922(15) . . ? C114 H115 2.075(16) . . ? C115 H114 1.99(2) . . ? C115 H116 2.056(19) . . ? C116 H115 2.065(9) . . ? C121 C123 2.397(12) . . ? C121 C124 2.763(11) . . ? C121 C125 2.396(9) . . ? C121 C0 2.897(9) . . ? C121 P2 3.731(6) . . ? C121 H116 2.630(6) . . ? C121 H122 2.023(5) . . ? C121 H126 2.048(4) . . ? C122 C124 2.391(10) . . ? C122 C125 2.722(7) . . ? C122 C126 2.341(7) . . ? C122 H123 2.082(8) . . ? C123 C125 2.331(9) . . ? C123 C126 2.721(10) . . ? C123 H122 2.058(8) . . ? C123 H124 2.029(7) . . ? C124 C126 2.354(12) . . ? C124 H123 2.018(7) . . ? C124 H125 2.006(7) . . ? C125 H124 1.999(9) . . ? C125 H126 2.058(9) . . ? C126 H125 2.053(7) . . ? C0 C211 2.855(9) . . ? C0 C221 2.843(9) . . ? C0 H212 2.627(5) . . ? P2 C212 2.834(8) . . ? P2 C216 2.717(9) . . ? P2 C222 2.795(6) . . ? P2 C226 2.795(8) . . ? P2 H0a 2.3358(14) . . ? P2 H0b 2.3352(16) . . ? P2 H212 2.9739(14) . . ? P2 H216 2.7781(16) . . ? P2 H222 2.8862(12) . . ? P2 H226 2.8904(16) . . ? C211 C213 2.396(12) . . ? C211 C214 2.767(14) . . ? C211 C215 2.416(12) . . ? C211 C221 2.833(10) . . ? C211 H212 2.037(7) . . ? C211 H216 2.035(7) . . ? C212 C214 2.349(15) . . ? C212 C215 2.699(13) . . ? C212 C216 2.321(12) . . ? C212 H213 2.082(8) . . ? C213 C215 2.289(16) . . ? C213 C216 2.709(13) . . ? C213 H212 2.050(12) . . ? C213 H214 2.038(12) . . ? C214 C216 2.387(15) . . ? C214 H213 1.931(13) . . ? C214 H215 2.090(13) . . ? C215 H214 1.941(13) . . ? C215 H216 2.120(13) . . ? C216 H215 2.096(9) . . ? C221 C223 2.408(9) . . ? C221 C224 2.778(12) . . ? C221 C225 2.413(13) . . ? C221 H222 2.047(5) . . ? C221 H226 2.035(5) . . ? C222 C224 2.378(14) . . ? C222 C225 2.736(12) . . ? C222 C226 2.357(8) . . ? C222 H223 2.068(6) . . ? C223 C225 2.313(11) . . ? C223 C226 2.715(8) . . ? C223 H222 2.080(10) . . ? C223 H224 1.977(11) . . ? C224 C226 2.386(10) . . ? C224 H223 2.015(10) . . ? C224 H225 2.016(9) . . ? C225 H224 2.021(8) . . ? C225 H226 2.073(9) . . ? C226 H225 2.073(8) . . ? C01 C03 2.245(12) . . ? C01 C04 2.225(17) . . ? C01 H02 2.129(13) . . ? C01 H05 2.148(15) . . ? C02 C04 2.253(17) . . ? C02 C05 2.238(16) . . ? C02 H01 2.142(12) . . ? C02 H03 2.138(14) . . ? C03 C05 2.203(16) . . ? C03 H02 2.152(12) . . ? C03 H04 2.076(12) . . ? C04 H03 2.103(11) . . ? C04 H05 2.034(11) . . ? C05 H01 2.032(17) . . ? C05 H04 2.108(17) . . ? C101 C103 2.30(2) . . ? C101 C104 2.77(2) . . ? C101 C105 2.46(2) . . ? C101 H102 1.879(18) . . ? C101 H106 2.128(18) . . ? C102 C104 2.38(3) . . ? C102 C105 2.63(2) . . ? C102 C106 2.28(3) . . ? C102 H101 1.94(2) . . ? C102 H103 2.08(2) . . ? C103 C105 2.17(3) . . ? C103 C106 2.64(3) . . ? C103 H102 2.02(2) . . ? C103 H104 2.10(2) . . ? C104 C106 2.33(2) . . ? C104 H103 1.94(2) . . ? C104 H105 1.916(19) . . ? C105 H104 1.81(2) . . ? C105 H106 2.18(2) . . ? C106 H101 2.13(3) . . ? C106 H105 2.06(2) . . ? H112 H113 2.39281(10) . . ? H112 H0b 2.21028(9) . . ? H113 H114 2.27938(10) . . ? H114 H115 2.30270(10) . . ? H115 H116 2.36404(10) . . ? H115 H215 2.10155(10) . 1_545 ? H122 H123 2.38746(10) . . ? H123 H124 2.30734(10) . . ? H124 H125 2.31058(13) . . ? H125 H126 2.34756(10) . . ? H126 H0a 2.23603(8) . . ? H0a H0b 1.55195(8) . . ? H0b H212 2.12008(8) . . ? H212 H213 2.39597(10) . . ? H213 H214 2.28760(12) . . ? H214 H215 2.31522(12) . . ? H215 H216 2.38141(10) . . ? H222 H223 2.37096(12) . . ? H223 H224 2.29250(12) . . ? H224 H225 2.32474(9) . . ? H225 H226 2.37977(12) . . ? H101 H102 2.21985(10) . . ? H102 H103 2.37937(11) . . ? H103 H104 2.35093(12) . . ? H104 H105 2.11767(9) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 W1 C12 78.9(3) . . . ? C11 W1 C13 78.0(3) . . . ? C11 W1 C1 131.7(3) . . . ? C11 W1 C01 145.1(4) . . . ? C11 W1 C02 127.4(5) . . . ? C11 W1 C03 93.8(4) . . . ? C11 W1 C04 87.6(4) . . . ? C11 W1 C05 115.1(5) . . . ? C12 W1 C13 110.7(4) . . . ? C12 W1 C1 77.0(2) . . . ? C12 W1 C01 123.8(4) . . . ? C12 W1 C02 96.6(4) . . . ? C12 W1 C03 102.5(4) . . . ? C12 W1 C04 134.5(4) . . . ? C12 W1 C05 154.4(4) . . . ? C13 W1 C1 72.5(3) . . . ? C13 W1 C01 111.7(4) . . . ? C13 W1 C02 146.7(3) . . . ? C13 W1 C03 143.2(4) . . . ? C13 W1 C04 108.5(4) . . . ? C13 W1 C05 93.7(4) . . . ? C1 W1 C01 82.3(3) . . . ? C1 W1 C02 96.6(4) . . . ? C1 W1 C03 132.0(3) . . . ? C1 W1 C04 137.6(3) . . . ? C1 W1 C05 104.3(5) . . . ? C01 W1 C02 35.0(4) . . . ? C01 W1 C03 57.8(3) . . . ? C01 W1 C04 57.4(4) . . . ? C01 W1 C05 34.2(5) . . . ? C02 W1 C03 35.5(5) . . . ? C02 W1 C04 58.6(5) . . . ? C02 W1 C05 57.8(4) . . . ? C03 W1 C04 34.8(4) . . . ? C03 W1 C05 57.2(5) . . . ? C04 W1 C05 34.2(5) . . . ? Co3 Co2 C21 147.4(3) . . . ? Co3 Co2 C22 99.5(2) . . . ? Co3 Co2 C3 50.76(16) . . . ? Co3 Co2 C4 51.17(14) . . . ? Co3 Co2 P1 96.01(5) . . . ? C21 Co2 C22 103.9(3) . . . ? C21 Co2 C3 97.3(3) . . . ? C21 Co2 C4 101.8(3) . . . ? C21 Co2 P1 95.95(18) . . . ? C22 Co2 C3 139.2(2) . . . ? C22 Co2 C4 100.5(2) . . . ? C22 Co2 P1 112.2(2) . . . ? C3 Co2 C4 40.44(17) . . . ? C3 Co2 P1 99.68(12) . . . ? C4 Co2 P1 137.69(13) . . . ? Co2 Co3 C31 148.8(3) . . . ? Co2 Co3 C32 99.6(2) . . . ? Co2 Co3 C3 51.19(16) . . . ? Co2 Co3 C4 50.51(14) . . . ? Co2 Co3 P2 96.79(5) . . . ? C31 Co3 C32 101.6(3) . . . ? C31 Co3 C3 99.5(3) . . . ? C31 Co3 C4 101.3(3) . . . ? C31 Co3 P2 97.23(17) . . . ? C32 Co3 C3 143.4(2) . . . ? C32 Co3 C4 105.8(2) . . . ? C32 Co3 P2 109.81(19) . . . ? C3 Co3 C4 40.37(17) . . . ? C3 Co3 P2 96.62(12) . . . ? C4 Co3 P2 135.21(14) . . . ? W1 C11 O11 178.0(8) . . . ? W1 C12 O12 177.1(8) . . . ? W1 C13 O13 177.6(8) . . . ? Co2 C21 O21 175.5(6) . . . ? Co2 C22 O22 175.9(6) . . . ? Co3 C31 O31 177.0(8) . . . ? Co3 C32 O32 178.9(6) . . . ? W1 C1 C2 174.5(4) . . . ? C1 C2 C3 176.1(5) . . . ? Co2 C3 Co3 78.1(2) . . . ? Co2 C3 C2 136.3(4) . . . ? Co2 C3 C4 69.0(3) . . . ? Co3 C3 C2 132.7(4) . . . ? Co3 C3 C4 70.2(3) . . . ? C2 C3 C4 142.2(5) . . . ? Co2 C4 Co3 78.32(18) . . . ? Co2 C4 C3 70.6(3) . . . ? Co2 C4 C4 134.1(3) . . 3_665 ? Co3 C4 C3 69.4(3) . . . ? Co3 C4 C4 134.6(4) . . 3_665 ? C3 C4 C4 141.8(6) . . 3_665 ? Co2 P1 C111 113.91(17) . . . ? Co2 P1 C121 122.97(17) . . . ? Co2 P1 C0 108.56(16) . . . ? C111 P1 C121 101.3(3) . . . ? C111 P1 C0 103.3(3) . . . ? C121 P1 C0 104.8(2) . . . ? P1 C111 C112 120.9(6) . . . ? P1 C111 C116 121.3(7) . . . ? C112 C111 C116 117.1(8) . . . ? C111 C112 C113 121.8(9) . . . ? C111 C112 H112 119.6(8) . . . ? C113 C112 H112 118.6(11) . . . ? C112 C113 C114 120.5(13) . . . ? C112 C113 H113 125.1(13) . . . ? C114 C113 H113 114.3(13) . . . ? C113 C114 C115 119.1(13) . . . ? C113 C114 H114 125.5(16) . . . ? C115 C114 H114 115.3(13) . . . ? C114 C115 C116 120.7(12) . . . ? C114 C115 H115 120.8(15) . . . ? C116 C115 H115 118.5(18) . . . ? C111 C116 C115 120.6(13) . . . ? C111 C116 H116 118.4(10) . . . ? C115 C116 H116 120.9(11) . . . ? P1 C121 C122 120.4(4) . . . ? P1 C121 C126 121.2(5) . . . ? C122 C121 C126 118.3(6) . . . ? C121 C122 C123 120.6(5) . . . ? C121 C122 H122 120.1(7) . . . ? C123 C122 H122 119.3(7) . . . ? C122 C123 C124 119.3(7) . . . ? C122 C123 H123 121.9(6) . . . ? C124 C123 H123 118.8(9) . . . ? C123 C124 C125 120.3(8) . . . ? C123 C124 H124 119.2(8) . . . ? C125 C124 H124 120.5(6) . . . ? C124 C125 C126 120.8(5) . . . ? C124 C125 H125 120.2(8) . . . ? C126 C125 H125 118.9(7) . . . ? C121 C126 C125 120.7(6) . . . ? C121 C126 H126 119.9(7) . . . ? C125 C126 H126 119.4(5) . . . ? P1 C0 P2 109.3(2) . . . ? P1 C0 H0a 110.6(4) . . . ? P1 C0 H0b 110.0(4) . . . ? P2 C0 H0a 109.7(4) . . . ? P2 C0 H0b 109.2(4) . . . ? H0a C0 H0b 108.1(4) . . . ? Co3 P2 C0 108.93(15) . . . ? Co3 P2 C211 115.72(18) . . . ? Co3 P2 C221 123.19(17) . . . ? C0 P2 C211 102.7(3) . . . ? C0 P2 C221 101.9(3) . . . ? C211 P2 C221 101.9(3) . . . ? P2 C211 C212 125.3(6) . . . ? P2 C211 C216 117.0(5) . . . ? C212 C211 C216 117.6(7) . . . ? C211 C212 C213 121.3(8) . . . ? C211 C212 H212 120.0(8) . . . ? C213 C212 H212 118.7(8) . . . ? C212 C213 C214 120.8(10) . . . ? C212 C213 H213 123.8(11) . . . ? C214 C213 H213 115.4(12) . . . ? C213 C214 C215 120.7(11) . . . ? C213 C214 H214 125.0(13) . . . ? C215 C214 H214 114.3(12) . . . ? C214 C215 C216 119.7(9) . . . ? C214 C215 H215 125.0(11) . . . ? C216 C215 H215 115.2(11) . . . ? C211 C216 C215 119.8(8) . . . ? C211 C216 H216 119.7(8) . . . ? C215 C216 H216 120.5(9) . . . ? P2 C221 C222 120.5(5) . . . ? P2 C221 C226 121.4(4) . . . ? C222 C221 C226 118.0(6) . . . ? C221 C222 C223 119.5(7) . . . ? C221 C222 H222 119.7(7) . . . ? C223 C222 H222 120.9(6) . . . ? C222 C223 C224 121.6(6) . . . ? C222 C223 H223 117.9(9) . . . ? C224 C223 H223 120.5(9) . . . ? C223 C224 C225 120.3(10) . . . ? C223 C224 H224 119.1(7) . . . ? C225 C224 H224 120.6(11) . . . ? C224 C225 C226 119.8(9) . . . ? C224 C225 H225 119.9(10) . . . ? C226 C225 H225 120.2(7) . . . ? C221 C226 C225 120.7(5) . . . ? C221 C226 H226 119.6(7) . . . ? C225 C226 H226 119.7(7) . . . ? W1 C01 C02 71.5(6) . . . ? W1 C01 C05 71.2(7) . . . ? W1 C01 H01 123.9(11) . . . ? C02 C01 C05 107.5(10) . . . ? C02 C01 H01 130.5(15) . . . ? C05 C01 H01 122.0(13) . . . ? W1 C02 C01 73.5(7) . . . ? W1 C02 C03 71.3(6) . . . ? W1 C02 H02 119.2(11) . . . ? C01 C02 C03 105.8(10) . . . ? C01 C02 H02 125.9(14) . . . ? C03 C02 H02 128.2(11) . . . ? W1 C03 C02 73.2(7) . . . ? W1 C03 C04 71.8(8) . . . ? W1 C03 H03 117.8(8) . . . ? C02 C03 C04 108.4(9) . . . ? C02 C03 H03 125.6(11) . . . ? C04 C03 H03 125.9(11) . . . ? W1 C04 C03 73.4(8) . . . ? W1 C04 C05 73.9(9) . . . ? W1 C04 H04 117.8(10) . . . ? C03 C04 C05 108.3(11) . . . ? C03 C04 H04 123.0(10) . . . ? C05 C04 H04 128.7(11) . . . ? W1 C05 C01 74.6(8) . . . ? W1 C05 C04 71.9(8) . . . ? W1 C05 H05 118.6(11) . . . ? C01 C05 C04 109.9(10) . . . ? C01 C05 H05 130.2(16) . . . ? C04 C05 H05 119.9(15) . . . ? C102 C101 C106 116.3(16) . . . ? C102 C101 H101 123.0(19) . . . ? C106 C101 H101 120.7(16) . . . ? C101 C102 C103 123.7(18) . . . ? C101 C102 H102 119(2) . . . ? C103 C102 H102 118(2) . . . ? C102 C103 C104 120.9(17) . . . ? C102 C103 H103 124(2) . . . ? C104 C103 H103 114.6(18) . . . ? C103 C104 C105 118.9(17) . . . ? C103 C104 H104 127.7(17) . . . ? C105 C104 H104 113(2) . . . ? C104 C105 C106 124.2(18) . . . ? C104 C105 H105 123(2) . . . ? C106 C105 H105 112(2) . . . ? C101 C106 C105 115.7(16) . . . ? C101 C106 H106 119.3(18) . . . ? C105 C106 H106 125(2) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -25 _reflns_limit_l_max 22 _reflns_number_total .108550+05 _reflns_number_observed 6205 _reflns_observed_criterion refl_observed_if_F____>4.000_sigma(F___) _reflns_d_resolution_high .73 _reflns_d_resolution_low 16.434 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 7.4844 _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_author ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 _publ_contact_author_fax (61)-8-9380-1005 _publ_contact_author_email bws@crystal.uwa.edu.au loop_ _publ_author_name _publ_author_address '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=END data_br620 _audit_creation_date 98-11-16 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common 'compound 4' _chemical_formula_analytical C56_H35_Co2_O10_P2_W2 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum C56_H35_Co2_O10_P2_W2 _chemical_formula_weight 1415.4 _chemical_melting_point ? _computing_data_collection 'Bruker SMART software' _computing_cell_refinement 'Bruker SAINT software' _computing_data_reduction 'BRUKER SAINT software' _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 13.656(2) _cell_length_b 14.520(2) _cell_length_c 15.450(2) _cell_angle_alpha 100.616(3) _cell_angle_beta 103.489(3) _cell_angle_gamma 113.166(3) _cell_volume 2605.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 5919 _cell_measurement_theta_min 0 _cell_measurement_theta_max 29 _cell_special_details ; ? ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _exptl_crystal_description plate _exptl_crystal_preparation ? _exptl_crystal_colour dark _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1366 _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 5.2 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.88 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device 'BRUKER CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 30621 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI .145 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.89 _diffrn_reflns_reduction_process ? loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 112 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 70 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Co ? 0 4 .299 .973 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 20 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 4 .09 .095 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 W ? 0 4 -1.421 6.872 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom W1 .44623(2) 1.60394(2) .173192(18) .04598(13) Uani ? ? W1' .69961(3) .94972(2) -.06476(2) .05668(15) Uani ? ? Co2 .65360(7) 1.61148(7) .39920(6) .0455(4) Uani ? ? Co3 .77106(7) 1.73003(7) .32736(6) .0473(4) Uani ? ? C11 .3541(7) 1.5153(7) .0419(6) .072(4) Uani ? ? O11 .2962(6) 1.4612(5) -.0329(4) .105(3) Uani ? ? C12 .4243(6) 1.4612(6) .1734(5) .059(3) Uani ? ? O12 .4089(5) 1.3784(4) .1745(4) .088(3) Uani ? ? C13 .5520(7) 1.6531(6) .1052(5) .064(4) Uani ? ? O13 .6115(6) 1.6875(5) .0649(4) .100(4) Uani ? ? C21 .5281(7) 1.5032(7) .3922(5) .064(4) Uani ? ? O21 .4484(5) 1.4347(5) .3875(4) .104(3) Uani ? ? C22 .6565(6) 1.7158(6) .4809(5) .058(3) Uani ? ? O22 .6553(5) 1.7848(5) .5313(4) .079(3) Uani ? ? C31 .8283(6) 1.7503(6) .2371(6) .064(4) Uani ? ? O31 .8710(5) 1.7653(5) .1821(4) .095(3) Uani ? ? C32 .7483(6) 1.8442(6) .3523(5) .056(3) Uani ? ? O32 .7249(5) 1.9112(4) .3606(4) .084(3) Uani ? ? C1 .6060(5) 1.6227(5) .2692(4) .043(3) Uani ? ? C2 .6761(5) 1.5770(5) .2794(4) .043(3) Uani ? ? C3 .6870(5) 1.4936(5) .2289(4) .046(3) Uani ? ? C4 .6985(6) 1.4214(6) .1885(5) .055(3) Uani ? ? C11' .8631(10) 1.0433(8) -.0127(8) .104(6) Uani ? ? O11' .9590(7) 1.0993(6) .0144(8) .174(6) Uani ? ? C12' .6414(8) .9183(7) .0368(6) .080(5) Uani ? ? O12' .6045(7) .9025(6) .0946(5) .125(5) Uani ? ? C13' .7630(7) .8515(6) -.0321(5) .067(4) Uani ? ? O13' .8008(5) .7978(5) -.0130(4) .087(3) Uani ? ? C1' .7148(6) 1.0929(6) .0134(6) .068(4) Uani ? ? C2' .7172(7) 1.1732(6) .0572(6) .069(4) Uani ? ? C3' .7131(6) 1.2606(6) .1023(5) .063(4) Uani ? ? C4' .7082(6) 1.3367(6) .1426(5) .062(3) Uani ? ? P1 .77791(15) 1.56308(15) .47396(12) .0516(8) Uani ? ? C111 .7336(6) 1.4220(6) .4430(5) .056(3) Uani ? ? C112 .6527(8) 1.3627(7) .4759(6) .077(4) Uani ? ? C113 .6135(9) 1.2547(8) .4552(7) .092(5) Uani ? ? C114 .6520(9) 1.2040(7) .3984(7) .089(5) Uani ? ? C115 .7291(8) 1.2606(7) .3616(6) .078(4) Uani ? ? C116 .7710(6) 1.3690(7) .3845(5) .069(4) Uani ? ? C121 .8354(6) 1.5989(6) .6019(5) .056(3) Uani ? ? C122 .9056(7) 1.5599(7) .6433(6) .079(4) Uani ? ? C123 .9528(8) 1.5910(9) .7402(7) .100(5) Uani ? ? C124 .9269(9) 1.6571(9) .7945(6) .097(5) Uani ? ? C125 .8587(7) 1.6953(7) .7550(6) .080(4) Uani ? ? C126 .8125(6) 1.6662(6) .6581(5) .064(4) Uani ? ? C0 .9051(6) 1.6188(6) .4425(5) .057(3) Uani ? ? P2 .92758(15) 1.74819(15) .43025(13) .0527(8) Uani ? ? C211 1.0574(6) 1.7876(6) .4005(5) .055(3) Uani ? ? C212 1.0604(7) 1.7191(6) .3223(6) .074(4) Uani ? ? C213 1.1559(9) 1.7478(9) .2994(7) .092(5) Uani ? ? C214 1.2480(8) 1.8419(10) .3479(8) .090(5) Uani ? ? C215 1.2466(7) 1.9098(7) .4191(7) .085(5) Uani ? ? C216 1.1511(7) 1.8829(6) .4464(6) .071(4) Uani ? ? C221 .9795(5) 1.8334(5) .5519(4) .053(3) Uani ? ? C222 1.0552(7) 1.8245(6) .6239(5) .073(4) Uani ? ? C223 1.0919(7) 1.8862(7) .7136(6) .078(4) Uani ? ? C224 1.0532(7) 1.9591(7) .7361(5) .079(4) Uani ? ? C225 .9787(7) 1.9696(6) .6659(6) .074(4) Uani ? ? C226 .9417(6) 1.9065(6) .5740(5) .062(3) Uani ? ? C01 .4512(7) 1.7224(7) .3041(5) .068(4) Uani ? ? C02 .3509(7) 1.6303(7) .2765(6) .073(4) Uani ? ? C03 .2861(6) 1.6179(7) .1844(5) .066(4) Uani ? ? C04 .3486(7) 1.7021(7) .1570(5) .064(4) Uani ? ? C05 .4512(6) 1.7680(6) .2305(6) .066(4) Uani ? ? C01' .6080(12) .9904(8) -.1877(7) .107(6) Uani ? ? C02' .6778(11) .9533(11) -.2181(7) .116(7) Uani ? ? C03' .6380(11) .8492(9) -.2200(6) .092(5) Uani ? ? C04' .5467(10) .8235(7) -.1899(7) .101(5) Uani ? ? C05' .5265(8) .9090(10) -.1687(6) .096(5) Uani ? ? C101 -.0695(11) .493(2) .0510(9) .126(8) Uani ? ? C102 -.0614(10) .4062(14) .0123(12) .126(8) Uani ? ? C103 .0090(14) .4124(13) -.0405(9) .129(8) Uani ? ? H112 .62224 1.39688 .51353 .09600 Uiso ? ? H113 .55793 1.21370 .48101 .11500 Uiso ? ? H114 .62601 1.12909 .38261 .10800 Uiso ? ? H115 .75293 1.22389 .31844 .09300 Uiso ? ? H116 .82746 1.40908 .35960 .08900 Uiso ? ? H122 .92195 1.51055 .60428 .09600 Uiso ? ? H123 1.00233 1.56365 .76850 .12500 Uiso ? ? H124 .95778 1.67655 .86208 .11800 Uiso ? ? H125 .84163 1.74433 .79443 .10300 Uiso ? ? H126 .76490 1.69554 .62995 .08100 Uiso ? ? H0a .97003 1.62594 .48915 .07100 Uiso ? ? H0b .89669 1.57350 .38401 .07100 Uiso ? ? H212 .99400 1.65140 .28683 .09100 Uiso ? ? H213 1.15818 1.70089 .24702 .11700 Uiso ? ? H214 1.31681 1.86238 .33049 .11100 Uiso ? ? H215 1.31291 1.97864 .45225 .11000 Uiso ? ? H216 1.15070 1.93153 .49872 .08900 Uiso ? ? H222 1.08496 1.77500 .60817 .09100 Uiso ? ? H223 1.14493 1.87947 .76297 .09600 Uiso ? ? H224 1.07943 2.00287 .80025 .09700 Uiso ? ? H225 .95138 2.02098 .68064 .09100 Uiso ? ? H226 .88855 1.91405 .52547 .07500 Uiso ? ? H01 .51129 1.75138 .36305 .08500 Uiso ? ? H02 .33029 1.58353 .31329 .09000 Uiso ? ? H03 .21203 1.56063 .14851 .08300 Uiso ? ? H04 .32594 1.71423 .09820 .08300 Uiso ? ? H05 .51276 1.83248 .23127 .08400 Uiso ? ? H01' .61426 1.06088 -.18110 .13700 Uiso ? ? H02' .74205 .99141 -.23537 .14600 Uiso ? ? H03' .66923 .80175 -.23787 .11600 Uiso ? ? H04' .50365 .75438 -.18455 .11900 Uiso ? ? H05' .46682 .91244 -.14572 .12500 Uiso ? ? H101 -.11913 .49333 .08769 .16000 Uiso ? ? H102 -.10620 .34374 .02475 .19400 Uiso ? ? H103 .01036 .34619 -.06871 .20400 Uiso ? ? 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 W1 .05153(18) .0527(2) .03704(15) .03103(15) .00844(13) .01296(13) W1' .0658(2) .04411(19) .0618(2) .02808(16) .02260(17) .01177(15) Co2 .0480(5) .0522(6) .0372(5) .0272(4) .0090(4) .0125(4) Co3 .0487(5) .0456(5) .0412(5) .0213(4) .0087(4) .0086(4) C11 .092(6) .082(6) .049(5) .060(5) .006(5) .012(4) O11 .134(6) .112(5) .050(4) .072(5) -.012(4) -.000(4) C12 .063(5) .056(5) .040(4) .025(4) -.002(3) .006(4) O12 .100(4) .048(3) .085(4) .026(3) -.002(3) .013(3) C13 .078(6) .079(6) .058(5) .053(5) .023(4) .027(4) O13 .112(5) .140(6) .103(5) .078(5) .066(4) .075(5) C21 .065(5) .081(6) .044(4) .035(5) .012(4) .022(4) O21 .070(4) .116(5) .082(4) .001(4) .019(4) .043(4) C22 .056(4) .072(5) .047(4) .035(4) .008(4) .017(4) O22 .104(4) .085(4) .061(3) .062(4) .027(3) .009(3) C31 .056(5) .052(5) .063(5) .013(4) .010(4) .007(4) O31 .088(4) .113(5) .073(4) .027(4) .039(4) .028(4) C32 .054(4) .052(5) .046(4) .018(4) .005(3) .004(4) O32 .084(4) .056(4) .102(5) .041(3) .010(3) .006(3) C1 .054(4) .038(4) .035(3) .020(3) .015(3) .011(3) C2 .043(4) .043(4) .045(4) .023(3) .012(3) .013(3) C3 .043(4) .047(4) .043(4) .020(3) .007(3) .012(3) C4 .063(5) .050(5) .057(5) .031(4) .021(4) .014(4) C11' .115(9) .064(6) .157(10) .046(6) .081(8) .028(7) O11' .085(5) .098(6) .288(12) .013(5) .079(7) -.005(7) C12' .104(7) .070(6) .085(7) .048(5) .049(6) .029(5) O12' .184(8) .113(6) .138(7) .084(6) .107(6) .064(5) C13' .070(5) .061(5) .065(5) .033(5) .017(4) .012(4) O13' .083(4) .091(5) .101(5) .056(4) .025(4) .035(4) C1' .070(5) .063(5) .075(6) .034(4) .030(4) .018(4) C2' .076(5) .064(5) .080(6) .039(5) .036(5) .020(5) C3' .072(5) .055(5) .072(5) .036(4) .033(4) .013(4) C4' .069(5) .060(5) .059(5) .032(4) .026(4) .016(4) P1 .0541(11) .0596(12) .0424(10) .0323(10) .0078(9) .0152(9) C111 .059(5) .058(5) .046(4) .032(4) .004(4) .013(4) C112 .101(7) .065(6) .073(6) .046(5) .026(5) .028(5) C113 .122(8) .071(7) .077(6) .040(6) .028(6) .028(5) C114 .106(8) .063(6) .080(7) .038(6) -.002(6) .023(5) C115 .086(6) .076(6) .069(6) .057(5) .001(5) .003(5) C116 .065(5) .069(6) .067(5) .040(5) .003(4) .015(4) C121 .058(4) .062(5) .045(4) .032(4) .004(4) .016(4) C122 .088(6) .097(7) .059(5) .059(5) .007(5) .024(5) C123 .109(8) .122(9) .067(6) .067(7) -.004(6) .033(6) C124 .111(8) .117(9) .049(5) .056(7) -.002(5) .022(6) C125 .091(6) .099(7) .050(5) .050(6) .019(5) .013(5) C126 .072(5) .083(6) .045(4) .046(5) .015(4) .020(4) C0 .060(4) .064(5) .051(4) .038(4) .011(4) .015(4) P2 .0467(10) .0572(12) .0486(11) .0261(9) .0092(9) .0077(9) C211 .055(4) .064(5) .053(4) .033(4) .017(4) .019(4) C212 .063(5) .061(5) .099(7) .027(4) .042(5) .011(5) C213 .089(7) .111(8) .105(8) .060(7) .058(6) .031(7) C214 .080(7) .118(9) .114(8) .060(7) .058(7) .062(7) C215 .067(6) .086(7) .104(8) .030(5) .032(6) .040(6) C216 .062(5) .068(6) .075(6) .028(5) .020(5) .017(5) C221 .045(4) .058(5) .043(4) .021(4) .007(3) .004(3) C222 .069(5) .079(6) .059(5) .042(5) -.001(4) .005(4) C223 .072(6) .083(6) .052(5) .031(5) -.009(4) .008(5) C224 .082(6) .072(6) .049(5) .024(5) .004(4) -.006(4) C225 .075(6) .062(5) .065(5) .032(5) .004(5) -.002(4) C226 .057(5) .062(5) .052(4) .026(4) .003(4) .004(4) C01 .066(5) .095(7) .046(4) .056(5) .007(4) -.001(4) C02 .080(6) .105(7) .055(5) .059(6) .030(5) .028(5) C03 .049(4) .092(6) .056(5) .040(4) .009(4) .010(4) C04 .069(5) .074(6) .061(5) .049(5) .012(4) .020(4) C05 .068(5) .063(5) .077(6) .045(4) .019(5) .014(4) C01' .156(11) .077(8) .078(7) .061(8) .007(7) .029(6) C02' .151(11) .134(11) .087(8) .066(9) .058(8) .064(8) C03' .139(10) .101(8) .061(6) .082(8) .031(6) .021(5) C04' .111(8) .070(7) .086(7) .041(6) -.007(6) .000(5) C05' .091(7) .117(9) .080(7) .072(7) -.001(6) .012(6) C101 .089(9) .221(18) .084(8) .079(13) .014(7) .082(11) C102 .061(7) .179(15) .121(11) .027(8) .009(7) .104(11) C103 .096(9) .166(13) .094(9) .045(9) -.012(7) .058(9) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls__F_____calc_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 7498 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .09 _refine_ls_R_factor_obs .04 _refine_ls_wR_factor_all .046 _refine_ls_wR_factor_obs .039 _refine_ls_goodness_of_fit_all .927 _refine_ls_goodness_of_fit_obs 1.038 _refine_ls_shift/esd_max .046 _refine_ls_shift/esd_mean .001 _refine_diff_density_min -1.148 _refine_diff_density_max 1.657 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C11 1.982(7) . . ? W1 C12 1.974(9) . . ? W1 C13 1.968(9) . . ? W1 C1 2.216(7) . . ? W1 C01 2.370(9) . . ? W1 C02 2.350(11) . . ? W1 C03 2.317(9) . . ? W1 C04 2.311(11) . . ? W1 C05 2.351(9) . . ? W1' C11' 1.962(11) . . ? W1' C12' 1.965(11) . . ? W1' C13' 2.018(11) . . ? W1' C1' 2.108(9) . . ? W1' C01' 2.325(13) . . ? W1' C02' 2.331(12) . . ? W1' C03' 2.323(9) . . ? W1' C04' 2.293(8) . . ? W1' C05' 2.302(10) . . ? Co2 Co3 2.4760(14) . . ? Co2 C21 1.775(8) . . ? Co2 C22 1.765(9) . . ? Co2 C1 2.019(7) . . ? Co2 C2 1.954(7) . . ? Co2 P1 2.243(3) . . ? Co3 C31 1.766(9) . . ? Co3 C32 1.795(10) . . ? Co3 C1 2.023(5) . . ? Co3 C2 1.961(6) . . ? Co3 P2 2.232(2) . . ? C11 O11 1.153(8) . . ? C12 O12 1.141(11) . . ? C13 O13 1.152(12) . . ? C21 O21 1.124(10) . . ? C22 O22 1.158(11) . . ? C31 O31 1.145(12) . . ? C32 O32 1.133(12) . . ? C1 C2 1.360(12) . . ? C2 C3 1.395(11) . . ? C3 C4 1.203(12) . . ? C4 C4' 1.372(13) . . ? C11' O11' 1.155(13) . . ? C12' O12' 1.140(15) . . ? C13' O13' 1.136(13) . . ? C1' C2' 1.220(13) . . ? C2' C3' 1.359(13) . . ? C3' C4' 1.198(13) . . ? P1 C111 1.822(8) . . ? P1 C121 1.836(7) . . ? P1 C0 1.827(8) . . ? C111 C112 1.376(13) . . ? C111 C116 1.393(13) . . ? C112 C113 1.386(14) . . ? C112 H112 .963(11) . . ? C113 C114 1.368(18) . . ? C113 H113 .981(11) . . ? C114 C115 1.370(15) . . ? C114 H114 .963(10) . . ? C115 C116 1.386(13) . . ? C115 H115 .970(11) . . ? C116 H116 .974(9) . . ? C121 C122 1.387(14) . . ? C121 C126 1.365(13) . . ? C122 C123 1.390(12) . . ? C122 H122 .978(11) . . ? C123 C124 1.364(18) . . ? C123 H123 .972(13) . . ? C124 C125 1.347(18) . . ? C124 H124 .969(9) . . ? C125 C126 1.390(11) . . ? C125 H125 .984(11) . . ? C126 H126 .974(10) . . ? C0 P2 1.834(9) . . ? C0 H0a .959(7) . . ? C0 H0b .968(7) . . ? P2 C211 1.833(9) . . ? P2 C221 1.843(6) . . ? C211 C212 1.437(12) . . ? C211 C216 1.371(9) . . ? C212 C213 1.356(16) . . ? C212 H212 .979(6) . . ? C213 C214 1.357(12) . . ? C213 H213 .973(12) . . ? C214 C215 1.344(17) . . ? C214 H214 .985(12) . . ? C215 C216 1.396(15) . . ? C215 H215 .982(7) . . ? C216 H216 .973(9) . . ? C221 C222 1.394(12) . . ? C221 C226 1.375(13) . . ? C222 C223 1.356(11) . . ? C222 H222 .977(11) . . ? C223 C224 1.382(16) . . ? C223 H223 .970(10) . . ? C224 C225 1.379(13) . . ? C224 H224 .969(8) . . ? C225 C226 1.390(11) . . ? C225 H225 .972(10) . . ? C226 H226 .970(8) . . ? C01 C02 1.386(11) . . ? C01 C05 1.416(14) . . ? C01 H01 .958(7) . . ? C02 C03 1.425(12) . . ? C02 H02 .965(10) . . ? C03 C04 1.393(12) . . ? C03 H03 .964(6) . . ? C04 C05 1.405(9) . . ? C04 H04 .960(9) . . ? C05 H05 .978(8) . . ? C01' C02' 1.39(2) . . ? C01' C05' 1.402(17) . . ? C01' H01' .977(13) . . ? C02' C03' 1.38(2) . . ? C02' H02' .964(14) . . ? C03' C04' 1.37(2) . . ? C03' H03' .974(16) . . ? C04' C05' 1.37(2) . . ? C04' H04' .974(10) . . ? C05' H05' .976(13) . . ? C101 C102 1.35(3) . . ? C101 H101 .982(17) . . ? C101 C103 1.36(3) . 2_565 ? C102 C103 1.39(3) . . ? C102 H102 .958(18) . . ? C103 H103 .99(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W1 Co2 3.9022(11) . . ? W1 Co3 3.9720(10) . . ? W1 O11 3.133(5) . . ? W1 O12 3.115(7) . . ? W1 O13 3.117(8) . . ? W1 C2 3.391(7) . . ? W1 H01 2.9917(5) . . ? W1 H02 2.9573(5) . . ? W1 H03 2.9206(6) . . ? W1 H04 2.9104(4) . . ? W1 H05 2.9652(5) . . ? W1' O11' 3.116(7) . . ? W1' O12' 3.104(9) . . ? W1' O13' 3.153(8) . . ? W1' C2' 3.326(9) . . ? W1' H01' 2.9609(5) . . ? W1' H02' 2.9454(5) . . ? W1' H03' 2.9335(5) . . ? W1' H04' 2.9008(4) . . ? W1' H05' 2.9164(6) . . ? Co2 O21 2.899(6) . . ? Co2 O22 2.921(7) . . ? Co2 C32 3.394(8) . . ? Co2 C3 3.095(8) . . ? Co2 C111 3.453(9) . . ? Co2 C121 3.598(8) . . ? Co2 C0 3.296(8) . . ? Co2 P2 3.337(2) . . ? Co3 C22 3.126(9) . . ? Co3 O31 2.909(7) . . ? Co3 O32 2.923(7) . . ? Co3 C3 3.095(7) . . ? Co3 P1 3.622(3) . . ? Co3 C0 3.314(9) . . ? Co3 C211 3.505(8) . . ? Co3 C221 3.536(6) . . ? Co3 H226 3.2257(9) . . ? C11 C12 2.436(13) . . ? C11 C13 2.460(10) . . ? C11 C03 2.962(14) . . ? C11 C04 2.995(14) . . ? C12 C1 2.506(8) . . ? O12 H04' 2.646(8) . 2_675 ? C13 C1 2.638(11) . . ? C21 C22 2.747(11) . . ? C21 C1 2.908(11) . . ? C21 C2 2.984(12) . . ? C21 P1 3.040(9) . . ? C22 H126 2.566(8) . . ? C22 H01 2.642(9) . . ? O22 H01 2.694(6) . . ? C31 C32 2.721(13) . . ? C31 C2 2.863(10) . . ? C31 P2 2.987(9) . . ? C32 C1 2.857(9) . . ? C32 H226 2.634(6) . . ? C1 C3 2.579(12) . . ? C2 C4 2.597(12) . . ? C2 P1 3.084(7) . . ? C3 C4' 2.575(12) . . ? C4 C3' 2.570(13) . . ? C11' C13' 2.494(13) . . ? C11' C1' 2.492(18) . . ? C12' C13' 2.558(16) . . ? C12' C1' 2.463(13) . . ? C13' C03' 2.992(14) . . ? C1' C3' 2.578(13) . . ? C1' C01' 2.910(12) . . ? C2' C4' 2.558(14) . . ? P1 C112 2.745(9) . . ? P1 C116 2.856(10) . . ? P1 C122 2.805(9) . . ? P1 C126 2.794(8) . . ? P1 P2 2.975(3) . . ? P1 H112 2.798(2) . . ? P1 H0a 2.350(2) . . ? P1 H0b 2.350(2) . . ? C111 C113 2.409(12) . . ? C111 C114 2.793(12) . . ? C111 C115 2.417(14) . . ? C111 C121 2.799(9) . . ? C111 C0 2.898(10) . . ? C111 H112 2.029(9) . . ? C111 H116 2.052(9) . . ? C112 C114 2.387(15) . . ? C112 C115 2.740(16) . . ? C112 C116 2.367(14) . . ? C112 H113 2.066(9) . . ? C113 C115 2.365(16) . . ? C113 C116 2.744(14) . . ? C113 H112 2.039(12) . . ? C113 H114 2.048(12) . . ? C114 C116 2.390(13) . . ? C114 H113 2.035(13) . . ? C114 H115 2.030(12) . . ? C115 H114 2.015(10) . . ? C115 H116 2.054(10) . . ? C116 H115 2.054(9) . . ? C121 C123 2.405(14) . . ? C121 C124 2.764(11) . . ? C121 C125 2.394(11) . . ? C121 C0 2.862(11) . . ? C121 H122 2.057(9) . . ? C121 H126 2.029(9) . . ? C122 C124 2.384(13) . . ? C122 C125 2.741(15) . . ? C122 C126 2.367(16) . . ? C122 H123 2.050(9) . . ? C123 C125 2.353(19) . . ? C123 C126 2.737(17) . . ? C123 H122 2.061(10) . . ? C123 H124 2.026(11) . . ? C124 C126 2.372(13) . . ? C124 H123 2.039(14) . . ? C124 H125 2.030(14) . . ? C125 H124 2.014(10) . . ? C125 H126 2.055(9) . . ? C126 H125 2.062(8) . . ? C0 C211 2.821(11) . . ? C0 C221 2.891(10) . . ? P2 C212 2.830(11) . . ? P2 C216 2.824(8) . . ? P2 C222 2.837(8) . . ? P2 C226 2.797(8) . . ? P2 H0a 2.340(2) . . ? P2 H0b 2.339(2) . . ? C211 C213 2.417(16) . . ? C211 C214 2.769(15) . . ? C211 C215 2.402(11) . . ? C211 C221 2.860(12) . . ? C211 H212 2.100(7) . . ? C211 H216 2.032(6) . . ? C212 C214 2.360(12) . . ? C212 C215 2.743(10) . . ? C212 C216 2.401(10) . . ? C212 H213 2.023(10) . . ? C213 C215 2.349(13) . . ? C213 C216 2.745(15) . . ? C213 H212 2.037(11) . . ? C213 H214 2.041(10) . . ? C214 C216 2.377(17) . . ? C214 H213 2.020(10) . . ? C214 H215 2.024(11) . . ? C215 H214 2.013(12) . . ? C215 H216 2.065(12) . . ? C216 H215 2.066(8) . . ? C221 C223 2.401(10) . . ? C221 C224 2.783(10) . . ? C221 C225 2.400(12) . . ? C221 H216 2.622(7) . . ? C221 H222 2.048(9) . . ? C221 H226 2.041(9) . . ? C222 C224 2.373(13) . . ? C222 C225 2.736(15) . . ? C222 C226 2.375(14) . . ? C222 H223 2.031(7) . . ? C223 C225 2.380(15) . . ? C223 C226 2.755(13) . . ? C223 H222 2.027(10) . . ? C223 H224 2.046(10) . . ? C224 C226 2.402(10) . . ? C224 H223 2.037(12) . . ? C224 H225 2.046(11) . . ? C225 H224 2.051(8) . . ? C225 H226 2.050(8) . . ? C226 H225 2.052(8) . . ? C01 C03 2.266(9) . . ? C01 C04 2.271(11) . . ? C01 H02 2.099(9) . . ? C01 H05 2.139(10) . . ? C02 C04 2.281(14) . . ? C02 C05 2.280(13) . . ? C02 H01 2.101(7) . . ? C02 H03 2.129(7) . . ? C03 C05 2.270(9) . . ? C03 H02 2.149(9) . . ? C03 H04 2.110(9) . . ? C04 H03 2.118(8) . . ? C04 H05 2.142(6) . . ? C05 H01 2.115(9) . . ? C05 H04 2.109(8) . . ? C01' C03' 2.24(2) . . ? C01' C04' 2.221(16) . . ? C01' H02' 2.123(17) . . ? C01' H05' 2.134(15) . . ? C02' C04' 2.228(17) . . ? C02' C05' 2.266(19) . . ? C02' H01' 2.118(18) . . ? C02' H03' 2.118(17) . . ? C03' C05' 2.25(2) . . ? C03' H02' 2.090(11) . . ? C03' H04' 2.079(12) . . ? C04' H03' 2.088(14) . . ? C04' H05' 2.110(14) . . ? C05' H01' 2.126(13) . . ? C05' H04' 2.100(14) . . ? C101 C101 2.71(2) . 2_565 ? C101 C102 2.36(2) . 2_565 ? C101 C103 2.36(3) . . ? C101 H102 1.96(3) . . ? C101 H103 2.09(3) . 2_565 ? C102 C102 2.73(3) . 2_565 ? C102 C103 2.36(3) . 2_565 ? C102 H101 2.06(2) . . ? C102 H103 2.03(2) . . ? C103 C103 2.75(3) . 2_565 ? C103 H101 1.982(17) . 2_565 ? C103 H102 2.088(18) . . ? H112 H113 2.3584(4) . . ? H113 H114 2.3569(2) . . ? H114 H115 2.3041(2) . . ? H115 H116 2.3634(4) . . ? H116 H0b 2.1123(3) . . ? H122 H123 2.3560(3) . . ? H123 H124 2.3387(2) . . ? H124 H125 2.3261(2) . . ? H125 H126 2.3597(3) . . ? H0a H0b 1.5514(2) . . ? H0a H222 2.2458(2) . . ? H0b H212 2.3819(2) . . ? H212 H213 2.3367(3) . . ? H213 H214 2.3324(2) . . ? H214 H215 2.3106(2) . . ? H215 H216 2.3709(3) . . ? H222 H223 2.3375(3) . . ? H223 H224 2.3374(2) . . ? H224 H225 2.3612(2) . . ? H225 H226 2.3484(3) . . ? H101 H102 2.3018(3) . . ? H101 H103 2.3353(3) . 2_565 ? H102 H103 2.3805(2) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 W1 C12 76.0(4) . . . ? C11 W1 C13 77.1(3) . . . ? C11 W1 C1 132.1(4) . . . ? C11 W1 C01 143.4(4) . . . ? C11 W1 C02 118.0(3) . . . ? C11 W1 C03 86.7(4) . . . ? C11 W1 C04 88.1(4) . . . ? C11 W1 C05 120.2(4) . . . ? C12 W1 C13 106.9(4) . . . ? C12 W1 C1 73.2(3) . . . ? C12 W1 C01 120.9(3) . . . ? C12 W1 C02 98.6(4) . . . ? C12 W1 C03 108.4(3) . . . ? C12 W1 C04 141.8(3) . . . ? C12 W1 C05 155.3(3) . . . ? C13 W1 C1 77.9(3) . . . ? C13 W1 C01 120.9(3) . . . ? C13 W1 C02 153.2(4) . . . ? C13 W1 C03 135.9(4) . . . ? C13 W1 C04 102.9(4) . . . ? C13 W1 C05 95.5(4) . . . ? C1 W1 C01 84.4(3) . . . ? C1 W1 C02 102.2(3) . . . ? C1 W1 C03 137.7(3) . . . ? C1 W1 C04 137.3(2) . . . ? C1 W1 C05 102.3(3) . . . ? C01 W1 C02 34.2(3) . . . ? C01 W1 C03 57.8(3) . . . ? C01 W1 C04 58.0(3) . . . ? C01 W1 C05 34.9(3) . . . ? C02 W1 C03 35.6(3) . . . ? C02 W1 C04 58.6(4) . . . ? C02 W1 C05 58.0(3) . . . ? C03 W1 C04 35.0(3) . . . ? C03 W1 C05 58.2(3) . . . ? C04 W1 C05 35.1(2) . . . ? C11' W1' C12' 109.7(4) . . . ? C11' W1' C13' 77.6(4) . . . ? C11' W1' C1' 75.4(4) . . . ? C11' W1' C01' 112.7(5) . . . ? C11' W1' C02' 96.4(5) . . . ? C11' W1' C03' 113.7(5) . . . ? C11' W1' C04' 148.3(5) . . . ? C11' W1' C05' 147.8(5) . . . ? C12' W1' C13' 79.9(4) . . . ? C12' W1' C1' 74.3(4) . . . ? C12' W1' C01' 123.5(5) . . . ? C12' W1' C02' 153.1(4) . . . ? C12' W1' C03' 130.3(4) . . . ? C12' W1' C04' 99.1(4) . . . ? C12' W1' C05' 94.8(4) . . . ? C13' W1' C1' 133.2(3) . . . ? C13' W1' C01' 144.3(4) . . . ? C13' W1' C02' 112.9(5) . . . ? C13' W1' C03' 86.9(4) . . . ? C13' W1' C04' 95.2(4) . . . ? C13' W1' C05' 128.7(4) . . . ? C1' W1' C01' 81.9(4) . . . ? C1' W1' C02' 107.5(5) . . . ? C1' W1' C03' 139.1(4) . . . ? C1' W1' C04' 126.7(4) . . . ? C1' W1' C05' 92.2(4) . . . ? C01' W1' C02' 34.8(6) . . . ? C01' W1' C03' 57.5(5) . . . ? C01' W1' C04' 57.5(4) . . . ? C01' W1' C05' 35.3(4) . . . ? C02' W1' C03' 34.6(5) . . . ? C02' W1' C04' 57.6(4) . . . ? C02' W1' C05' 58.6(5) . . . ? C03' W1' C04' 34.6(5) . . . ? C03' W1' C05' 58.2(5) . . . ? C04' W1' C05' 34.8(5) . . . ? Co3 Co2 C21 151.8(2) . . . ? Co3 Co2 C22 93.4(3) . . . ? Co3 Co2 C1 52.28(17) . . . ? Co3 Co2 C2 50.88(18) . . . ? Co3 Co2 P1 100.14(7) . . . ? C21 Co2 C22 101.8(4) . . . ? C21 Co2 C1 99.9(3) . . . ? C21 Co2 C2 106.2(3) . . . ? C21 Co2 P1 97.6(3) . . . ? C22 Co2 C1 109.6(4) . . . ? C22 Co2 C2 141.5(4) . . . ? C22 Co2 P1 107.8(3) . . . ? C1 Co2 C2 40.0(3) . . . ? C1 Co2 P1 134.1(2) . . . ? C2 Co2 P1 94.3(2) . . . ? Co2 Co3 C31 150.9(2) . . . ? Co2 Co3 C32 104.1(3) . . . ? Co2 Co3 C1 52.2(2) . . . ? Co2 Co3 C2 50.7(2) . . . ? Co2 Co3 P2 90.13(7) . . . ? C31 Co3 C32 99.7(4) . . . ? C31 Co3 C1 108.8(3) . . . ? C31 Co3 C2 100.3(3) . . . ? C31 Co3 P2 96.0(3) . . . ? C32 Co3 C1 96.7(3) . . . ? C32 Co3 C2 136.3(3) . . . ? C32 Co3 P2 112.9(2) . . . ? C1 Co3 C2 39.9(3) . . . ? C1 Co3 P2 137.5(2) . . . ? C2 Co3 P2 103.2(2) . . . ? W1 C11 O11 176.6(8) . . . ? W1 C12 O12 178.0(8) . . . ? W1 C13 O13 175.0(10) . . . ? Co2 C21 O21 179.8(9) . . . ? Co2 C22 O22 177.0(8) . . . ? Co3 C31 O31 176.3(7) . . . ? Co3 C32 O32 173.4(5) . . . ? W1 C1 Co2 134.2(4) . . . ? W1 C1 Co3 139.1(4) . . . ? W1 C1 C2 141.9(4) . . . ? Co2 C1 Co3 75.6(2) . . . ? Co2 C1 C2 67.4(4) . . . ? Co3 C1 C2 67.6(3) . . . ? Co2 C2 Co3 78.5(2) . . . ? Co2 C2 C1 72.6(4) . . . ? Co2 C2 C3 134.4(6) . . . ? Co3 C2 C1 72.5(4) . . . ? Co3 C2 C3 133.8(5) . . . ? C1 C2 C3 138.8(5) . . . ? C2 C3 C4 177.6(8) . . . ? C3 C4 C4' 178.1(8) . . . ? W1' C11' O11' 177.1(12) . . . ? W1' C12' O12' 176.6(11) . . . ? W1' C13' O13' 178.6(6) . . . ? W1' C1' C2' 176.5(7) . . . ? C1' C2' C3' 176.4(9) . . . ? C2' C3' C4' 178.9(9) . . . ? C4 C4' C3' 177.8(8) . . . ? Co2 P1 C111 115.9(2) . . . ? Co2 P1 C121 123.5(3) . . . ? Co2 P1 C0 107.7(3) . . . ? C111 P1 C121 99.8(4) . . . ? C111 P1 C0 105.2(4) . . . ? C121 P1 C0 102.7(3) . . . ? P1 C111 C112 117.6(7) . . . ? P1 C111 C116 124.8(6) . . . ? C112 C111 C116 117.5(8) . . . ? C111 C112 C113 121.5(10) . . . ? C111 C112 H112 119.2(9) . . . ? C113 C112 H112 119.3(10) . . . ? C112 C113 C114 120.2(10) . . . ? C112 C113 H113 120.6(12) . . . ? C114 C113 H113 119.1(10) . . . ? C113 C114 C115 119.5(10) . . . ? C113 C114 H114 122.0(11) . . . ? C115 C114 H114 118.4(12) . . . ? C114 C115 C116 120.3(10) . . . ? C114 C115 H115 119.3(10) . . . ? C116 C115 H115 120.3(10) . . . ? C111 C116 C115 120.9(8) . . . ? C111 C116 H116 119.1(8) . . . ? C115 C116 H116 120.0(10) . . . ? P1 C121 C122 120.4(7) . . . ? P1 C121 C126 120.9(7) . . . ? C122 C121 C126 118.7(7) . . . ? C121 C122 C123 120.0(10) . . . ? C121 C122 H122 120.0(8) . . . ? C123 C122 H122 120.0(11) . . . ? C122 C123 C124 119.9(12) . . . ? C122 C123 H123 119.4(12) . . . ? C124 C123 H123 120.7(10) . . . ? C123 C124 C125 120.5(9) . . . ? C123 C124 H124 119.6(13) . . . ? C125 C124 H124 119.9(12) . . . ? C124 C125 C126 120.2(10) . . . ? C124 C125 H125 120.2(8) . . . ? C126 C125 H125 119.6(10) . . . ? C121 C126 C125 120.7(9) . . . ? C121 C126 H126 119.5(7) . . . ? C125 C126 H126 119.8(9) . . . ? P1 C0 P2 108.7(5) . . . ? P1 C0 H0a 111.2(6) . . . ? P1 C0 H0b 110.6(4) . . . ? P2 C0 H0a 109.8(5) . . . ? P2 C0 H0b 109.3(6) . . . ? H0a C0 H0b 107.2(9) . . . ? Co3 P2 C0 108.8(2) . . . ? Co3 P2 C211 118.8(3) . . . ? Co3 P2 C221 120.1(3) . . . ? C0 P2 C211 100.6(4) . . . ? C0 P2 C221 103.7(3) . . . ? C211 P2 C221 102.2(3) . . . ? P2 C211 C212 119.4(5) . . . ? P2 C211 C216 123.0(7) . . . ? C212 C211 C216 117.5(8) . . . ? C211 C212 C213 119.8(6) . . . ? C211 C212 H212 119.6(9) . . . ? C213 C212 H212 120.6(9) . . . ? C212 C213 C214 120.9(11) . . . ? C212 C213 H213 119.7(8) . . . ? C214 C213 H213 119.4(12) . . . ? C213 C214 C215 120.9(11) . . . ? C213 C214 H214 120.4(12) . . . ? C215 C214 H214 118.7(9) . . . ? C214 C215 C216 120.3(8) . . . ? C214 C215 H215 120.1(11) . . . ? C216 C215 H215 119.6(10) . . . ? C211 C216 C215 120.5(9) . . . ? C211 C216 H216 119.3(9) . . . ? C215 C216 H216 120.3(7) . . . ? P2 C221 C222 121.8(7) . . . ? P2 C221 C226 120.1(5) . . . ? C222 C221 C226 118.1(7) . . . ? C221 C222 C223 121.7(10) . . . ? C221 C222 H222 118.5(7) . . . ? C223 C222 H222 119.8(9) . . . ? C222 C223 C224 120.2(9) . . . ? C222 C223 H223 120.7(11) . . . ? C224 C223 H223 119.0(8) . . . ? C223 C224 C225 119.2(7) . . . ? C223 C224 H224 120.0(9) . . . ? C225 C224 H224 120.8(11) . . . ? C224 C225 C226 120.4(9) . . . ? C224 C225 H225 120.0(8) . . . ? C226 C225 H225 119.6(9) . . . ? C221 C226 C225 120.4(8) . . . ? C221 C226 H226 120.0(7) . . . ? C225 C226 H226 119.6(9) . . . ? W1 C01 C02 72.1(6) . . . ? W1 C01 C05 71.8(5) . . . ? W1 C01 H01 122.1(9) . . . ? C02 C01 C05 108.9(7) . . . ? C02 C01 H01 126.3(10) . . . ? C05 C01 H01 124.8(8) . . . ? W1 C02 C01 73.7(6) . . . ? W1 C02 C03 71.0(5) . . . ? W1 C02 H02 120.4(9) . . . ? C01 C02 C03 107.4(8) . . . ? C01 C02 H02 125.5(8) . . . ? C03 C02 H02 127.1(7) . . . ? W1 C03 C02 73.5(6) . . . ? W1 C03 C04 72.2(6) . . . ? W1 C03 H03 120.0(7) . . . ? C02 C03 C04 108.0(6) . . . ? C02 C03 H03 124.9(9) . . . ? C04 C03 H03 127.0(8) . . . ? W1 C04 C03 72.7(6) . . . ? W1 C04 C05 74.0(6) . . . ? W1 C04 H04 119.9(8) . . . ? C03 C04 C05 108.5(8) . . . ? C03 C04 H04 126.4(6) . . . ? C05 C04 H04 125.1(8) . . . ? W1 C05 C01 73.3(6) . . . ? W1 C05 C04 70.9(6) . . . ? W1 C05 H05 120.1(8) . . . ? C01 C05 C04 107.2(7) . . . ? C01 C05 H05 125.6(7) . . . ? C04 C05 H05 127.1(9) . . . ? W1' C01' C02' 72.8(8) . . . ? W1' C01' C05' 71.5(7) . . . ? W1' C01' H01' 122.0(7) . . . ? C02' C01' C05' 108.4(12) . . . ? C02' C01' H01' 125.8(14) . . . ? C05' C01' H01' 125.7(17) . . . ? W1' C02' C01' 72.4(7) . . . ? W1' C02' C03' 72.4(7) . . . ? W1' C02' H02' 121.0(8) . . . ? C01' C02' C03' 107.4(12) . . . ? C01' C02' H02' 127.7(16) . . . ? C03' C02' H02' 125.0(17) . . . ? W1' C03' C02' 73.1(6) . . . ? W1' C03' C04' 71.5(6) . . . ? W1' C03' H03' 120.0(8) . . . ? C02' C03' C04' 108.0(13) . . . ? C02' C03' H03' 127.1(13) . . . ? C04' C03' H03' 124.9(12) . . . ? W1' C04' C03' 73.9(5) . . . ? W1' C04' C05' 73.0(5) . . . ? W1' C04' H04' 119.7(8) . . . ? C03' C04' C05' 109.9(10) . . . ? C03' C04' H04' 124.0(14) . . . ? C05' C04' H04' 126.1(13) . . . ? W1' C05' C01' 73.3(7) . . . ? W1' C05' C04' 72.3(7) . . . ? W1' C05' H05' 120.1(7) . . . ? C01' C05' C04' 106.3(12) . . . ? C01' C05' H05' 126.7(15) . . . ? C04' C05' H05' 127.0(12) . . . ? C102 C101 H101 124(2) . . . ? C102 C101 C103 121.6(17) . . 2_565 ? H101 C101 C103 115(3) . . 2_565 ? C101 C102 C103 119.9(17) . . . ? C101 C102 H102 115.2(18) . . . ? C103 C102 H102 125(2) . . . ? C102 C103 H103 116.6(17) . . . ? C102 C103 C101 119(2) . . 2_565 ? H103 C103 C101 124.8(19) . . 2_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min -19 _reflns_limit_k_max 17 _reflns_limit_l_min -20 _reflns_limit_l_max 19 _reflns_number_total .127860+05 _reflns_number_observed 7498 _reflns_observed_criterion refl_observed_if_F____>4.000_sigma(F___) _reflns_d_resolution_high .735 _reflns_d_resolution_low 14.249 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 14.0896 _publ_flag ? ? ? ? ? ? ? ? ? ? _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_author ; B.W.Skelton, A.H.White University of Western Australia Department of Chemistry Nedlands Western Australia 6907 Australia ; _publ_contact_letter ; ? letter to co-editor ; _publ_contact_author_phone (61)-8-9380-3144 _publ_contact_author_fax (61)-8-9380-1005 _publ_contact_author_email bws@crystal.uwa.edu.au loop_ _publ_author_name _publ_author_address '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ?