#------------------------------------------------------------------------------ #$Date: 2019-10-08 06:42:58 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219151 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234447.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7234447 loop_ _publ_author_name 'Su, Yan-Hui' 'Jia, Jia-Ge' 'Huang, Xin-Da' 'Feng, Jian-Shen' 'Bao, Song-Song' 'Ren, Min' 'Kurmoo, Mohamedally' 'Zheng, Li-Min' _publ_section_title ; Changes in magnetic order through two consecutive dehydration steps of metal-phosphonate diamond chains ; _journal_issue 55 _journal_name_full 'RSC Advances' _journal_page_first 31911 _journal_paper_doi 10.1039/C9RA05722F _journal_volume 9 _journal_year 2019 _chemical_formula_moiety 'C12 H36 Co3 N2 O20 P4, 4(H2 O)' _chemical_formula_sum 'C12 H44 Co3 N2 O24 P4' _chemical_formula_weight 901.16 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-06-05 deposited with the CCDC. 2019-09-30 downloaded from the CCDC. ; _cell_angle_alpha 114.883(6) _cell_angle_beta 97.803(7) _cell_angle_gamma 90.634(6) _cell_formula_units_Z 1 _cell_length_a 9.064(4) _cell_length_b 9.536(4) _cell_length_c 9.686(4) _cell_measurement_reflns_used 2450 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.08 _cell_measurement_theta_min 2.27 _cell_volume 750.3(6) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_unetI/netI 0.0195 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 11991 _diffrn_reflns_point_group_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.996 _diffrn_reflns_theta_min 2.275 _exptl_absorpt_coefficient_mu 1.953 _exptl_absorpt_correction_T_max 0.829 _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.994 _exptl_crystal_description block _exptl_crystal_F_000 463 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.580 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.113 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 2853 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0374 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1188 _refine_ls_wR_factor_ref 0.1223 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2638 _reflns_number_total 2853 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra05722f2.cif _cod_data_source_block Co-1 _cod_original_cell_volume 750.3(5) _cod_database_code 7234447 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.696 _shelx_estimated_absorpt_t_max 0.829 _shelx_res_file ; TITL Ni in P-1 Co-1.res created by SHELXL-2018/3 at 14:19:33 on 05-Jun-2019 CELL 0.71073 9.0639 9.5362 9.6861 114.883 97.803 90.634 ZERR 1.00 0.0035 0.0037 0.0037 0.006 0.007 0.006 LATT 1 SFAC C H N O P Co UNIT 12 44 2 24 4 3 OMIT -1 4 0 OMIT 0 -2 4 OMIT -1 -3 1 OMIT -2 52 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 HTAB O5W O3_$3 HTAB O5W O2_$3 HTAB O5W O2_$5 HTAB O4W O7_$4 HTAB O4W O7_$9 HTAB O3W O5W_$8 HTAB O3W O4W_$7 HTAB O2W O6_$6 HTAB O1W O6 HTAB O1W O4 HTAB O1W O3W_$6 HTAB N1 O5_$4 HTAB N1 O5W HTAB C6 O3 HTAB C5 O4W HTAB C5 O7_$4 HTAB C4 O4_$3 HTAB C3 O7 HTAB C2 O2 HTAB CONF size 0.20 0.15 0.10 HTAB C2 O2 HTAB C3 O7 EQIV $3 x-1, y, z HTAB C4 O4_$3 EQIV $4 -x+1, -y+1, -z+1 HTAB C5 O7_$4 HTAB C5 O4W EQIV $5 -x+1, -y+1, -z+2 HTAB C5 O5W_$5 HTAB C6 O3 HTAB N1 O5W HTAB N1 O5_$4 EQIV $6 -x+2, -y+2, -z+1 HTAB O1W O3W_$6 HTAB O1W O4 HTAB O1W O6 HTAB O2W O6_$6 EQIV $7 x, y+1, z HTAB O3W O4W_$7 EQIV $8 -x+1, -y+2, -z+2 HTAB O3W O5W_$8 EQIV $9 x, y-1, z HTAB O4W O7_$9 HTAB O4W O7_$4 HTAB O5W O2_$5 HTAB O5W O2_$3 HTAB O5W O3_$3 WGHT 0.105000 FVAR 0.61210 CO1 6 1.000000 0.500000 0.500000 10.50000 0.01563 0.01250 = 0.01094 0.00215 0.00268 0.00232 CO2 6 0.969660 1.057183 0.787048 11.00000 0.02046 0.01196 = 0.01096 0.00427 0.00183 -0.00118 P1 5 0.966295 0.758584 0.843586 11.00000 0.01194 0.01003 = 0.00957 0.00363 0.00149 0.00111 P2 5 0.760935 0.770648 0.571891 11.00000 0.01530 0.01111 = 0.01000 0.00367 0.00059 0.00089 C1 1 0.778591 0.804591 0.776305 11.00000 0.01480 0.00725 = 0.01024 0.00064 0.00184 0.00181 C2 1 0.652508 0.731101 0.821441 11.00000 0.01398 0.01463 = 0.01474 0.00656 0.00266 0.00211 AFIX 13 H2 2 0.680513 0.756983 0.931215 11.00000 -1.20000 AFIX 0 C3 1 0.498455 0.792396 0.803987 11.00000 0.01487 0.02309 = 0.03290 0.01203 0.00550 0.00314 AFIX 23 H3A 2 0.507058 0.904755 0.855666 11.00000 -1.20000 H3B 2 0.461766 0.761669 0.695711 11.00000 -1.20000 AFIX 0 C4 1 0.389785 0.729419 0.872200 11.00000 0.01837 0.02661 = 0.02939 0.00763 0.00704 0.00259 AFIX 23 H4A 2 0.422051 0.767827 0.982282 11.00000 -1.20000 H4B 2 0.292043 0.765430 0.856242 11.00000 -1.20000 AFIX 0 C5 1 0.526086 0.491868 0.807775 11.00000 0.02373 0.02124 = 0.03079 0.01461 0.00586 -0.00357 AFIX 23 H5A 2 0.513839 0.379766 0.752855 11.00000 -1.20000 H5B 2 0.566004 0.518119 0.914502 11.00000 -1.20000 AFIX 0 C6 1 0.635911 0.554901 0.738128 11.00000 0.01899 0.01395 = 0.02178 0.00414 0.00461 -0.00112 AFIX 23 H6A 2 0.732168 0.513674 0.747786 11.00000 -1.20000 H6B 2 0.599976 0.522901 0.629496 11.00000 -1.20000 AFIX 0 N1 3 0.379248 0.555877 0.799802 11.00000 0.02004 0.02630 = 0.01808 0.00587 0.00138 -0.00846 AFIX 23 H1A 2 0.320023 0.521861 0.847165 11.00000 -1.20000 H1B 2 0.337665 0.521208 0.701551 11.00000 -1.20000 AFIX 0 O1 4 0.780505 0.974029 0.859260 11.00000 0.01777 0.00658 = 0.01576 0.00157 0.00467 0.00326 AFIX 3 H1C 2 0.722304 1.026919 0.920370 11.00000 -1.20000 AFIX 0 O2 4 0.960325 0.767981 1.004586 11.00000 0.02000 0.01397 = 0.01223 0.00595 0.00252 -0.00087 O3 4 1.003890 0.597403 0.737728 11.00000 0.01967 0.01309 = 0.01294 0.00353 0.00266 0.00336 O4 4 1.071152 0.889092 0.848678 11.00000 0.01422 0.01488 = 0.01640 0.00748 0.00247 0.00009 O5 4 0.801063 0.605102 0.480553 11.00000 0.02046 0.01324 = 0.01405 0.00288 0.00046 0.00235 O6 4 0.880226 0.890402 0.577442 11.00000 0.02621 0.01685 = 0.01250 0.00560 0.00170 -0.00590 O7 4 0.605597 0.800663 0.518145 11.00000 0.02065 0.02699 = 0.02010 0.01168 -0.00120 0.00718 O1W 4 1.135898 0.697569 0.518999 11.00000 0.03699 0.01879 = 0.02778 0.00375 0.01489 0.00131 AFIX 3 H1WB 2 1.113118 0.711719 0.437969 11.00000 -1.50000 H1WA 2 1.119358 0.777659 0.596789 11.00000 -1.50000 AFIX 0 O2W 4 1.154137 1.103967 0.698957 11.00000 0.03092 0.05881 = 0.02694 0.02695 0.00372 -0.00678 AFIX 3 H2WA 2 1.222607 1.045647 0.704867 11.00000 -1.50000 H2WB 2 1.128337 1.087647 0.605427 11.00000 -1.50000 AFIX 0 O3W 4 0.828692 1.228913 0.749914 11.00000 0.04109 0.02389 = 0.02444 0.00951 -0.00389 0.00245 AFIX 3 H3WB 2 0.752662 1.183093 0.682604 11.00000 -1.50000 H3WA 2 0.800442 1.289653 0.833594 11.00000 -1.50000 AFIX 0 O4W 4 0.523175 0.105099 0.695406 11.00000 0.10243 0.03050 = 0.03114 0.01036 -0.00971 0.02625 AFIX 3 H4WA 2 0.536995 0.003549 0.646796 11.00000 -1.20000 H4WB 2 0.450645 0.134999 0.642676 11.00000 -1.20000 AFIX 0 O5W 4 0.159192 0.489765 0.952498 11.00000 0.02106 0.03123 = 0.04270 0.02385 0.00405 0.00130 AFIX 3 H5WA 2 0.129682 0.401925 0.957709 11.00000 -1.20000 H5WB 2 0.094372 0.512905 0.887457 11.00000 -1.20000 AFIX 0 HKLF 4 REM Ni in P-1 REM wR2 = 0.1223, GooF = S = 1.005, Restrained GooF = 1.005 for all data REM R1 = 0.0374 for 2638 Fo > 4sig(Fo) and 0.0398 for all 2853 data REM 205 parameters refined using 0 restraints END WGHT 0.0669 0.8517 REM Instructions for potential hydrogen bonds HTAB C2 O2 HTAB C3 O7 HTAB C4 O4_$3 HTAB C5 O7_$4 HTAB C5 O4W HTAB C6 O3 HTAB N1 O5W HTAB N1 O5_$4 HTAB O1W O3W_$6 HTAB O1W O4 HTAB O1W O6 HTAB O2W O6_$6 HTAB O3W O4W_$7 HTAB O3W O5W_$8 HTAB O4W O7_$9 HTAB O4W O7_$4 HTAB O5W O2_$5 HTAB O5W O2_$3 HTAB O5W O3_$3 REM Highest difference peak 0.580, deepest hole -0.835, 1-sigma level 0.113 Q1 1 0.8212 1.0050 0.9638 11.00000 0.05 0.58 Q2 1 0.9097 0.9854 0.7001 11.00000 0.05 0.55 Q3 1 1.0615 0.5614 0.5850 11.00000 0.05 0.53 Q4 1 1.0285 1.1338 0.8818 11.00000 0.05 0.53 Q5 1 1.0666 0.5039 0.4556 11.00000 0.05 0.47 ; _shelx_res_checksum 99319 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Co1 Co 1.000000 0.500000 0.500000 0.01393(17) Uani 1 2 d S . P Co2 Co 0.96966(4) 1.05718(4) 0.78705(4) 0.01475(16) Uani 1 1 d . . . P1 P 0.96629(7) 0.75858(7) 0.84359(7) 0.01072(19) Uani 1 1 d . . . P2 P 0.76093(7) 0.77065(8) 0.57189(8) 0.01257(19) Uani 1 1 d . . . C1 C 0.7786(3) 0.8046(3) 0.7763(3) 0.0118(5) Uani 1 1 d . . . C2 C 0.6525(3) 0.7311(3) 0.8214(3) 0.0143(5) Uani 1 1 d . . . H2 H 0.680513 0.756983 0.931215 0.017 Uiso 1 1 calc R U . C3 C 0.4985(3) 0.7924(4) 0.8040(4) 0.0234(6) Uani 1 1 d . . . H3A H 0.507058 0.904755 0.855666 0.028 Uiso 1 1 calc R U . H3B H 0.461766 0.761669 0.695711 0.028 Uiso 1 1 calc R U . C4 C 0.3898(3) 0.7294(4) 0.8722(4) 0.0259(7) Uani 1 1 d . . . H4A H 0.422051 0.767827 0.982282 0.031 Uiso 1 1 calc R U . H4B H 0.292043 0.765430 0.856242 0.031 Uiso 1 1 calc R U . C5 C 0.5261(3) 0.4919(4) 0.8078(4) 0.0239(6) Uani 1 1 d . . . H5A H 0.513839 0.379766 0.752855 0.029 Uiso 1 1 calc R U . H5B H 0.566004 0.518119 0.914502 0.029 Uiso 1 1 calc R U . C6 C 0.6359(3) 0.5549(3) 0.7381(3) 0.0193(6) Uani 1 1 d . . . H6A H 0.732168 0.513674 0.747786 0.023 Uiso 1 1 calc R U . H6B H 0.599976 0.522901 0.629496 0.023 Uiso 1 1 calc R U . N1 N 0.3792(3) 0.5559(3) 0.7998(3) 0.0230(5) Uani 1 1 d . . . H1A H 0.320023 0.521861 0.847165 0.028 Uiso 1 1 calc R U . H1B H 0.337665 0.521208 0.701551 0.028 Uiso 1 1 calc R U . O1 O 0.7805(2) 0.9740(2) 0.8593(2) 0.0142(4) Uani 1 1 d . . . H1C H 0.722304 1.026919 0.920370 0.017 Uiso 1 1 d R U . O2 O 0.9603(2) 0.7680(2) 1.0046(2) 0.0153(4) Uani 1 1 d . . . O3 O 1.0039(2) 0.5974(2) 0.7377(2) 0.0159(4) Uani 1 1 d . . . O4 O 1.07115(19) 0.8891(2) 0.8487(2) 0.0149(4) Uani 1 1 d . . . O5 O 0.8011(2) 0.6051(2) 0.4806(2) 0.0172(4) Uani 1 1 d . . . O6 O 0.8802(2) 0.8904(2) 0.5774(2) 0.0189(4) Uani 1 1 d . . . O7 O 0.6056(2) 0.8007(2) 0.5181(2) 0.0224(5) Uani 1 1 d . . . O1W O 1.1359(3) 0.6976(3) 0.5190(3) 0.0290(5) Uani 1 1 d . . . H1WB H 1.113118 0.711719 0.437969 0.043 Uiso 1 1 d R U . H1WA H 1.119358 0.777659 0.596789 0.043 Uiso 1 1 d R U . O2W O 1.1541(3) 1.1040(3) 0.6990(3) 0.0361(6) Uani 1 1 d . . . H2WA H 1.222607 1.045647 0.704867 0.054 Uiso 1 1 d R U . H2WB H 1.128337 1.087647 0.605427 0.054 Uiso 1 1 d R U . O3W O 0.8287(3) 1.2289(3) 0.7499(3) 0.0310(5) Uani 1 1 d . . . H3WB H 0.752662 1.183093 0.682604 0.046 Uiso 1 1 d R U . H3WA H 0.800442 1.289653 0.833594 0.046 Uiso 1 1 d R U . O4W O 0.5232(4) 0.1051(3) 0.6954(3) 0.0575(9) Uani 1 1 d . . . H4WA H 0.536995 0.003549 0.646796 0.069 Uiso 1 1 d R U . H4WB H 0.450645 0.134999 0.642676 0.069 Uiso 1 1 d R U . O5W O 0.1592(2) 0.4898(3) 0.9525(3) 0.0290(5) Uani 1 1 d . . . H5WA H 0.129682 0.401925 0.957709 0.035 Uiso 1 1 d R U . H5WB H 0.094372 0.512905 0.887457 0.035 Uiso 1 1 d R U . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0156(3) 0.0125(3) 0.0109(3) 0.0021(2) 0.0027(2) 0.0023(2) Co2 0.0205(2) 0.0120(2) 0.0110(2) 0.00427(18) 0.00183(16) -0.00118(16) P1 0.0119(3) 0.0100(4) 0.0096(4) 0.0036(3) 0.0015(2) 0.0011(3) P2 0.0153(3) 0.0111(4) 0.0100(3) 0.0037(3) 0.0006(3) 0.0009(3) C1 0.0148(12) 0.0073(12) 0.0102(12) 0.0006(10) 0.0018(10) 0.0018(9) C2 0.0140(12) 0.0146(13) 0.0147(13) 0.0066(11) 0.0027(10) 0.0021(10) C3 0.0149(13) 0.0231(15) 0.0329(17) 0.0120(14) 0.0055(12) 0.0031(11) C4 0.0184(14) 0.0266(16) 0.0294(17) 0.0076(14) 0.0070(12) 0.0026(12) C5 0.0237(14) 0.0212(15) 0.0308(17) 0.0146(14) 0.0059(12) -0.0036(12) C6 0.0190(13) 0.0140(14) 0.0218(14) 0.0041(12) 0.0046(11) -0.0011(10) N1 0.0200(12) 0.0263(14) 0.0181(12) 0.0059(11) 0.0014(10) -0.0085(10) O1 0.0178(9) 0.0066(9) 0.0158(9) 0.0016(8) 0.0047(7) 0.0033(7) O2 0.0200(9) 0.0140(9) 0.0122(9) 0.0059(8) 0.0025(7) -0.0009(7) O3 0.0197(9) 0.0131(9) 0.0129(9) 0.0035(8) 0.0027(7) 0.0034(7) O4 0.0142(9) 0.0149(10) 0.0164(10) 0.0075(8) 0.0025(7) 0.0001(7) O5 0.0205(10) 0.0132(10) 0.0140(10) 0.0029(8) 0.0005(7) 0.0023(7) O6 0.0262(10) 0.0168(10) 0.0125(9) 0.0056(8) 0.0017(8) -0.0059(8) O7 0.0207(10) 0.0270(11) 0.0201(11) 0.0117(9) -0.0012(8) 0.0072(8) O1W 0.0370(12) 0.0188(11) 0.0278(12) 0.0037(10) 0.0149(10) 0.0013(9) O2W 0.0309(12) 0.0588(16) 0.0269(12) 0.0269(12) 0.0037(10) -0.0068(11) O3W 0.0411(13) 0.0239(12) 0.0244(12) 0.0095(10) -0.0039(10) 0.0025(10) O4W 0.102(2) 0.0305(15) 0.0311(15) 0.0104(12) -0.0097(15) 0.0263(16) O5W 0.0211(10) 0.0312(12) 0.0427(14) 0.0239(11) 0.0040(9) 0.0013(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O3 Co1 O3 180.0 . 2_766 O3 Co1 O5 91.56(7) . 2_766 O3 Co1 O5 88.44(7) 2_766 2_766 O3 Co1 O5 88.44(7) . . O3 Co1 O5 91.56(7) 2_766 . O5 Co1 O5 180.0 2_766 . O3 Co1 O1W 91.01(8) . . O3 Co1 O1W 88.99(8) 2_766 . O5 Co1 O1W 87.54(9) 2_766 . O5 Co1 O1W 92.46(9) . . O3 Co1 O1W 88.99(8) . 2_766 O3 Co1 O1W 91.01(8) 2_766 2_766 O5 Co1 O1W 92.46(9) 2_766 2_766 O5 Co1 O1W 87.54(9) . 2_766 O1W Co1 O1W 180.0 . 2_766 O2 Co2 O6 174.52(7) 2_777 . O2 Co2 O2W 91.57(9) 2_777 . O6 Co2 O2W 91.64(9) . . O2 Co2 O4 93.38(8) 2_777 . O6 Co2 O4 90.76(8) . . O2W Co2 O4 94.88(9) . . O2 Co2 O1 94.79(7) 2_777 . O6 Co2 O1 82.40(8) . . O2W Co2 O1 172.00(9) . . O4 Co2 O1 79.92(7) . . O2 Co2 O3W 84.20(8) 2_777 . O6 Co2 O3W 91.02(9) . . O2W Co2 O3W 96.62(10) . . O4 Co2 O3W 168.31(8) . . O1 Co2 O3W 88.86(8) . . O3 P1 O2 109.80(11) . . O3 P1 O4 113.43(11) . . O2 P1 O4 112.00(11) . . O3 P1 C1 111.89(11) . . O2 P1 C1 106.09(11) . . O4 P1 C1 103.26(11) . . O7 P2 O5 113.34(12) . . O7 P2 O6 112.20(12) . . O5 P2 O6 111.27(11) . . O7 P2 C1 109.63(11) . . O5 P2 C1 107.42(11) . . O6 P2 C1 102.28(11) . . O1 C1 C2 108.50(19) . . O1 C1 P2 103.53(16) . . C2 C1 P2 116.81(18) . . O1 C1 P1 104.13(15) . . C2 C1 P1 111.97(17) . . P2 C1 P1 110.74(13) . . C6 C2 C3 108.4(2) . . C6 C2 C1 113.4(2) . . C3 C2 C1 115.3(2) . . C6 C2 H2 106.4 . . C3 C2 H2 106.4 . . C1 C2 H2 106.4 . . C4 C3 C2 110.4(2) . . C4 C3 H3A 109.6 . . C2 C3 H3A 109.6 . . C4 C3 H3B 109.6 . . C2 C3 H3B 109.6 . . H3A C3 H3B 108.1 . . N1 C4 C3 110.9(2) . . N1 C4 H4A 109.5 . . C3 C4 H4A 109.5 . . N1 C4 H4B 109.5 . . C3 C4 H4B 109.5 . . H4A C4 H4B 108.0 . . N1 C5 C6 111.5(2) . . N1 C5 H5A 109.3 . . C6 C5 H5A 109.3 . . N1 C5 H5B 109.3 . . C6 C5 H5B 109.3 . . H5A C5 H5B 108.0 . . C2 C6 C5 109.5(2) . . C2 C6 H6A 109.8 . . C5 C6 H6A 109.8 . . C2 C6 H6B 109.8 . . C5 C6 H6B 109.8 . . H6A C6 H6B 108.2 . . C5 N1 C4 112.7(2) . . C5 N1 H1A 109.0 . . C4 N1 H1A 109.0 . . C5 N1 H1B 109.0 . . C4 N1 H1B 109.0 . . H1A N1 H1B 107.8 . . C1 O1 Co2 103.26(13) . . C1 O1 H1C 128.3 . . Co2 O1 H1C 128.5 . . P1 O2 Co2 129.76(11) . 2_777 P1 O3 Co1 128.95(11) . . P1 O4 Co2 116.51(10) . . P2 O5 Co1 130.18(11) . . P2 O6 Co2 117.74(11) . . Co1 O1W H1WB 109.2 . . Co1 O1W H1WA 109.2 . . H1WB O1W H1WA 109.5 . . Co2 O2W H2WA 109.5 . . Co2 O2W H2WB 109.9 . . H2WA O2W H2WB 109.5 . . Co2 O3W H3WB 110.0 . . Co2 O3W H3WA 110.4 . . H3WB O3W H3WA 109.5 . . H4WA O4W H4WB 112.5 . . H5WA O5W H5WB 112.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 O3 2.084(2) . Co1 O3 2.084(2) 2_766 Co1 O5 2.0971(19) 2_766 Co1 O5 2.0971(19) . Co1 O1W 2.167(2) . Co1 O1W 2.167(2) 2_766 Co2 O2 2.013(2) 2_777 Co2 O6 2.029(2) . Co2 O2W 2.101(2) . Co2 O4 2.1121(19) . Co2 O1 2.1954(19) . Co2 O3W 2.205(2) . P1 O3 1.5199(19) . P1 O2 1.5324(19) . P1 O4 1.5376(19) . P1 C1 1.862(3) . P2 O7 1.507(2) . P2 O5 1.527(2) . P2 O6 1.543(2) . P2 C1 1.850(3) . C1 O1 1.470(3) . C1 C2 1.538(3) . C2 C6 1.522(4) . C2 C3 1.535(4) . C2 H2 0.9800 . C3 C4 1.505(4) . C3 H3A 0.9700 . C3 H3B 0.9700 . C4 N1 1.497(4) . C4 H4A 0.9700 . C4 H4B 0.9700 . C5 N1 1.476(4) . C5 C6 1.522(4) . C5 H5A 0.9700 . C5 H5B 0.9700 . C6 H6A 0.9700 . C6 H6B 0.9700 . N1 H1A 0.8900 . N1 H1B 0.8900 . O1 H1C 0.8500 . O1W H1WB 0.8501 . O1W H1WA 0.8500 . O2W H2WA 0.8500 . O2W H2WB 0.8501 . O3W H3WB 0.8500 . O3W H3WA 0.8500 . O4W H4WA 0.9001 . O4W H4WB 0.8999 . O5W H5WA 0.9000 . O5W H5WB 0.9001 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O5W H5WB O3 0.90 2.02 2.898(3) 163.0 1_455 yes O5W H5WB O2 0.90 2.61 3.126(3) 117.4 1_455 yes O5W H5WA O2 0.90 1.99 2.883(3) 169.4 2_667 yes O4W H4WB O7 0.90 1.91 2.717(3) 147.8 2_666 yes O4W H4WA O7 0.90 1.97 2.852(3) 165.3 1_545 yes O3W H3WA O5W 0.85 2.23 2.986(3) 148.7 2_677 yes O3W H3WB O4W 0.85 2.24 2.889(4) 133.4 1_565 yes O2W H2WB O6 0.85 1.86 2.676(3) 160.2 2_776 yes O1W H1WA O6 0.85 2.45 2.941(3) 117.5 . yes O1W H1WA O4 0.85 2.32 3.083(3) 149.2 . yes O1W H1WB O3W 0.85 2.24 3.023(3) 152.5 2_776 yes N1 H1B O5 0.89 1.93 2.763(3) 155.4 2_666 yes N1 H1A O5W 0.89 1.98 2.850(3) 165.6 . yes C6 H6A O3 0.97 2.61 3.356(3) 134.1 . yes C5 H5A O4W 0.97 2.44 3.376(4) 161.4 . yes C5 H5A O7 0.97 2.53 3.266(4) 132.4 2_666 yes C4 H4B O4 0.97 2.34 3.305(4) 171.1 1_455 yes C3 H3B O7 0.97 2.44 3.087(4) 124.2 . yes C2 H2 O2 0.98 2.53 3.027(3) 111.5 . yes C2 H2 O2 0.98 2.53 3.027(3) 111.5 . yes C3 H3B O7 0.97 2.44 3.087(4) 124.2 . yes C4 H4B O4 0.97 2.34 3.305(4) 171.1 1_455 yes C5 H5A O7 0.97 2.53 3.266(4) 132.4 2_666 yes C5 H5A O4W 0.97 2.44 3.376(4) 161.4 . yes C5 H5B O5W 0.97 2.66 3.378(4) 130.9 2_667 yes C6 H6A O3 0.97 2.61 3.356(3) 134.1 . yes N1 H1A O5W 0.89 1.98 2.850(3) 165.6 . yes N1 H1B O5 0.89 1.93 2.763(3) 155.4 2_666 yes O1W H1WB O3W 0.85 2.24 3.023(3) 152.5 2_776 yes O1W H1WA O4 0.85 2.32 3.083(3) 149.2 . yes O1W H1WA O6 0.85 2.45 2.941(3) 117.5 . yes O2W H2WB O6 0.85 1.86 2.676(3) 160.2 2_776 yes O3W H3WB O4W 0.85 2.24 2.889(4) 133.4 1_565 yes O3W H3WA O5W 0.85 2.23 2.986(3) 148.7 2_677 yes O4W H4WA O7 0.90 1.97 2.852(3) 165.3 1_545 yes O4W H4WB O7 0.90 1.91 2.717(3) 147.8 2_666 yes O5W H5WA O2 0.90 1.99 2.883(3) 169.4 2_667 yes O5W H5WB O2 0.90 2.61 3.126(3) 117.4 1_455 yes O5W H5WB O3 0.90 2.02 2.898(3) 163.0 1_455 yes 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_4 O7 P2 C1 O1 -71.88(17) . O5 P2 C1 O1 164.57(14) . O6 P2 C1 O1 47.35(17) . O7 P2 C1 C2 47.3(2) . O5 P2 C1 C2 -76.3(2) . O6 P2 C1 C2 166.51(18) . O7 P2 C1 P1 177.05(12) . O5 P2 C1 P1 53.49(16) . O6 P2 C1 P1 -63.72(15) . O3 P1 C1 O1 -162.99(14) . O2 P1 C1 O1 77.28(17) . O4 P1 C1 O1 -40.65(17) . O3 P1 C1 C2 80.0(2) . O2 P1 C1 C2 -39.7(2) . O4 P1 C1 C2 -157.67(18) . O3 P1 C1 P2 -52.31(16) . O2 P1 C1 P2 -172.03(12) . O4 P1 C1 P2 70.04(14) . O1 C1 C2 C6 178.0(2) . P2 C1 C2 C6 61.6(3) . P1 C1 C2 C6 -67.6(3) . O1 C1 C2 C3 52.2(3) . P2 C1 C2 C3 -64.2(3) . P1 C1 C2 C3 166.59(19) . C6 C2 C3 C4 59.7(3) . C1 C2 C3 C4 -172.0(3) . C2 C3 C4 N1 -56.6(3) . C3 C2 C6 C5 -59.4(3) . C1 C2 C6 C5 171.2(2) . N1 C5 C6 C2 57.6(3) . C6 C5 N1 C4 -54.8(3) . C3 C4 N1 C5 54.3(3) . C2 C1 O1 Co2 178.21(16) . P2 C1 O1 Co2 -57.06(14) . P1 C1 O1 Co2 58.80(14) . O3 P1 O2 Co2 141.37(13) 2_777 O4 P1 O2 Co2 14.41(17) 2_777 C1 P1 O2 Co2 -97.55(15) 2_777 O2 P1 O3 Co1 170.64(12) . O4 P1 O3 Co1 -63.21(16) . C1 P1 O3 Co1 53.12(17) . O3 P1 O4 Co2 122.39(11) . O2 P1 O4 Co2 -112.63(12) . C1 P1 O4 Co2 1.09(14) . O7 P2 O5 Co1 178.47(13) . O6 P2 O5 Co1 50.90(17) . C1 P2 O5 Co1 -60.28(17) . O7 P2 O6 Co2 104.66(14) . O5 P2 O6 Co2 -127.16(12) . C1 P2 O6 Co2 -12.74(15) .