#------------------------------------------------------------------------------ #$Date: 2019-10-08 06:42:39 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219150 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234443.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_7234443 loop_ _publ_author_name 'Rojek, Tomasz' 'Goldeman, Waldemar' '\'Slepokura, Katarzyna' 'Duczmal, Marek' 'Wojciechowska, Agnieszka' 'Matczak-Jon, Ewa' _publ_section_title ; Low pH constructed Co(ii) and Ni(ii) 1D coordination polymers based on C\a-substituted analogues of zoledronic acid: structural characterization, and spectroscopic and magnetic properties ; _journal_issue 54 _journal_name_full 'RSC Advances' _journal_page_first 31497 _journal_paper_doi 10.1039/C9RA05673D _journal_volume 9 _journal_year 2019 _chemical_formula_moiety 'C7 H12 Co N2 O8 P2, (H2 O)' _chemical_formula_sum 'C7 H14 Co N2 O9 P2' _chemical_formula_weight 391.07 _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 _atom_sites_solution_primary isomor _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-09-11 deposited with the CCDC. 2019-09-24 downloaded from the CCDC. ; _cell_angle_alpha 90.97(3) _cell_angle_beta 93.60(3) _cell_angle_gamma 114.95(3) _cell_formula_units_Z 2 _cell_length_a 7.848(3) _cell_length_b 7.886(3) _cell_length_c 10.880(5) _cell_measurement_reflns_used 3450 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 28.77 _cell_measurement_theta_min 2.84 _cell_volume 608.6(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'DIAMOND ver. 3.2 (Brandenburg, Putz, 2006)' _computing_publication_material 'PLATON (Spek, 2009)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean 10.3456 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Agilent Technologies, Xcalibur R, Ruby' _diffrn_measurement_method 'omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0658 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.948 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 16719 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.948 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.840 _diffrn_reflns_theta_min 1.878 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.726 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour pink _exptl_crystal_density_diffrn 2.134 _exptl_crystal_description column _exptl_crystal_F_000 398 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.507 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 5098 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 0.924 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0325 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.0639 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3840 _reflns_number_total 5098 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra05673d2.cif _cod_data_source_block tr21116ab _cod_database_code 7234443 _shelx_shelxl_version_number 2014/7 _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 0.820 _shelx_estimated_absorpt_t_max 0.934 _shelx_res_file ; tr21116ab.res created by SHELXL-2014/7 TITL tr21116 in P-1 CELL 0.71073 7.848 7.886 10.880 90.97 93.60 114.95 ZERR 2 0.003 0.003 0.005 0.03 0.03 0.03 LATT 1 SFAC C H Co N O P UNIT 14 28 2 4 18 4 L.S. 10 PLAN 20 temp -163 size 0.12 0.04 0.04 EQIV $1 1-X,1-Y,1-Z EQIV $2 +X,1+Y,+Z EQIV $3 -1+X,+Y,+Z EQIV $4 1-X,1-Y,2-Z EQIV $5 2-X,2-Y,2-Z EQIV $6 2-X,2-Y,1-Z EQIV $7 2-X,1-Y,1-Z HTAB O3 O5 HTAB O7 O6_$1 HTAB C3 O5_$2 HTAB C4 O3_$3 HTAB N2 O5_$4 HTAB C21 O2W_$1 HTAB C41 O1_$5 HTAB C41 O3_$5 HTAB C51 O2W_$6 HTAB O1W O2_$7 HTAB O1W O6_$7 HTAB O2W O5_$7 HTAB O2W O1_$6 HTAB O2W O1W CONF BOND $H HTAB fmap 2 acta DFIX 0.84 0.002 o1w h1w o1w h2w O2W H3w O2W H4w o7 h7 DFIX 1.36 0.002 H1W h2w h3w h4w WGHT 0.031800 BASF 0.34994 FVAR 2.53648 CO1 3 0.813001 0.675940 0.432630 11.00000 0.00646 0.00605 = 0.00661 0.00054 0.00130 0.00212 P1 6 0.959937 0.904546 0.677603 11.00000 0.00490 0.00531 = 0.00647 0.00004 0.00055 0.00130 P2 6 0.620925 0.531937 0.681279 11.00000 0.00680 0.00424 = 0.00619 0.00048 0.00098 0.00186 O1 5 1.040092 1.114034 0.682784 11.00000 0.00622 0.00406 = 0.00962 0.00001 0.00143 -0.00104 O2 5 1.017559 0.811027 0.576029 11.00000 0.00629 0.00760 = 0.00859 -0.00017 -0.00019 0.00261 O3 5 1.011355 0.849811 0.809176 11.00000 0.00736 0.00608 = 0.01148 0.00278 0.00055 -0.00050 AFIX 147 H3 2 0.936620 0.739055 0.821275 11.00000 -1.50000 AFIX 0 O4 5 0.409961 0.443498 0.693311 11.00000 0.00624 0.00678 = 0.00716 -0.00072 0.00236 -0.00026 O5 5 0.732496 0.518246 0.797434 11.00000 0.00702 0.00712 = 0.00825 0.00087 0.00151 0.00256 O6 5 0.675600 0.462508 0.563542 11.00000 0.00887 0.00570 = 0.00777 -0.00052 0.00259 0.00254 O7 5 0.659072 0.807226 0.528275 11.00000 0.00664 0.00646 = 0.00296 0.00103 -0.00003 0.00152 AFIX 3 H7 2 0.549450 0.725340 0.509042 11.00000 -1.50000 AFIX 0 C1 1 0.696937 0.786627 0.657718 11.00000 0.00468 0.00615 = 0.00573 0.00105 -0.00015 0.00160 C2 1 0.598977 0.879629 0.733720 11.00000 0.00620 0.00637 = 0.00495 0.00125 0.00129 0.00294 C3 1 0.625852 1.074590 0.706788 11.00000 0.01430 0.01026 = 0.01169 0.00179 0.00283 0.00859 AFIX 23 H3A 2 0.638821 1.160875 0.777550 11.00000 -1.20000 H3B 2 0.701396 1.134572 0.637215 11.00000 -1.20000 AFIX 0 C4 1 0.437582 0.913910 0.676983 11.00000 0.00872 0.01636 = 0.01127 -0.00008 0.00157 0.00814 AFIX 23 H4A 2 0.397168 0.874773 0.589068 11.00000 -1.20000 H4B 2 0.334582 0.901081 0.729426 11.00000 -1.20000 AFIX 0 N1 4 0.582502 0.831650 0.862397 11.00000 0.00857 0.00706 = 0.00740 0.00132 0.00196 0.00371 N2 4 0.467876 0.685522 1.023906 11.00000 0.01265 0.00630 = 0.00868 0.00092 0.00484 0.00217 AFIX 43 H2 2 0.390457 0.605210 1.072306 11.00000 -1.20000 AFIX 0 C21 1 0.432988 0.693454 0.904820 11.00000 0.01154 0.00909 = 0.00829 -0.00120 0.00379 0.00545 AFIX 43 H21 2 0.320677 0.614419 0.857153 11.00000 -1.20000 AFIX 0 C41 1 0.643674 0.821813 1.061132 11.00000 0.01382 0.01306 = 0.01034 -0.00399 -0.00243 0.00657 AFIX 43 H41 2 0.703101 0.845302 1.142351 11.00000 -1.20000 AFIX 0 C51 1 0.716236 0.916289 0.960343 11.00000 0.00629 0.00955 = 0.00844 -0.00246 -0.00002 0.00150 AFIX 43 H51 2 0.835181 1.020032 0.957210 11.00000 -1.20000 AFIX 0 O1W 5 0.948496 0.517743 0.361399 11.00000 0.00997 0.00878 = 0.02220 0.00290 0.00416 0.00460 AFIX 3 H1W 2 1.066372 0.573490 0.372027 11.00000 -1.50000 H2W 2 0.915552 0.406291 0.380608 11.00000 -1.50000 AFIX 0 O2W 5 0.976361 0.645313 0.096853 11.00000 0.03446 0.04110 = 0.03760 0.00301 0.00522 0.01472 AFIX 3 H3W 2 1.054966 0.602635 0.118544 11.00000 -1.50000 H4W 2 0.940952 0.677138 0.161280 11.00000 -1.50000 AFIX 0 HKLF 5 REM tr21116 in P-1 REM R1 = 0.0325 for 3840 Fo > 4sig(Fo) and 0.0499 for all 5098 data REM 192 parameters refined using 7 restraints END WGHT 0.0318 0.0000 REM Instructions for potential hydrogen bonds HTAB O3 O5 HTAB O7 O6_$1 HTAB C3 O5_$2 HTAB C4 O3_$3 HTAB N2 O5_$4 HTAB C21 O2W_$1 HTAB C41 O1_$5 HTAB C41 O3_$5 HTAB C51 O2W_$6 HTAB O1W O6_$7 HTAB O1W O2_$7 HTAB O2W O5_$7 HTAB O2W O1_$6 HTAB O2W O1W REM Highest difference peak 0.507, deepest hole -0.588, 1-sigma level 0.101 Q1 1 0.6366 0.6639 0.6713 11.00000 0.05 0.51 Q2 1 0.4958 0.5287 0.6747 11.00000 0.05 0.45 Q3 1 0.5013 0.4364 0.6995 11.00000 0.05 0.44 Q4 1 0.3275 0.3449 0.6254 11.00000 0.05 0.42 Q5 1 1.0674 1.0341 0.6656 11.00000 0.05 0.39 Q6 1 0.7906 0.8203 0.6435 11.00000 0.05 0.38 Q7 1 0.6011 0.4316 0.5026 11.00000 0.05 0.38 Q8 1 0.5810 0.8597 0.8024 11.00000 0.05 0.38 Q9 1 0.9894 0.9035 0.4798 11.00000 0.05 0.37 Q10 1 0.5867 0.7289 1.0396 11.00000 0.05 0.37 Q11 1 0.9796 0.8493 0.7388 11.00000 0.05 0.37 Q12 1 0.8023 0.5467 0.4437 11.00000 0.05 0.36 Q13 1 0.9841 1.0308 0.6950 11.00000 0.05 0.36 Q14 1 0.7832 0.9573 0.5257 11.00000 0.05 0.36 Q15 1 0.6865 0.8776 0.5651 11.00000 0.05 0.35 Q16 1 0.9616 1.0438 0.6055 11.00000 0.05 0.34 Q17 1 0.4079 0.4469 0.7475 11.00000 0.05 0.34 Q18 1 0.6658 0.9344 1.0005 11.00000 0.05 0.33 Q19 1 0.7077 0.5296 0.5167 11.00000 0.05 0.33 Q20 1 0.3336 0.8148 0.6015 11.00000 0.05 0.32 ; _shelx_res_checksum 13727 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 Co1 Co 0.81300(6) 0.67594(5) 0.43263(3) 0.00651(10) Uani 1 1 d . . P1 P 0.95994(10) 0.90455(10) 0.67760(7) 0.00585(16) Uani 1 1 d . . P2 P 0.62092(10) 0.53194(10) 0.68128(7) 0.00588(16) Uani 1 1 d . . O1 O 1.0401(3) 1.1140(2) 0.68278(18) 0.0077(4) Uani 1 1 d . . O2 O 1.0176(2) 0.8110(2) 0.57603(18) 0.0076(4) Uani 1 1 d . . O3 O 1.0114(3) 0.8498(3) 0.80918(18) 0.0094(4) Uani 1 1 d . . H3 H 0.9366 0.7391 0.8213 0.014 Uiso 1 1 calc R U O4 O 0.4100(2) 0.4435(2) 0.69331(18) 0.0077(4) Uani 1 1 d . . O5 O 0.7325(2) 0.5182(2) 0.79743(17) 0.0076(4) Uani 1 1 d . . O6 O 0.6756(3) 0.4625(2) 0.56354(18) 0.0076(4) Uani 1 1 d . . O7 O 0.6591(2) 0.8072(2) 0.52827(15) 0.0058(4) Uani 1 1 d D . H7 H 0.5495 0.7253 0.5090 0.009 Uiso 1 1 d DR U C1 C 0.6969(4) 0.7866(4) 0.6577(2) 0.0058(6) Uani 1 1 d . . C2 C 0.5990(4) 0.8796(3) 0.7337(2) 0.0057(6) Uani 1 1 d . . C3 C 0.6259(4) 1.0746(4) 0.7068(3) 0.0108(6) Uani 1 1 d . . H3A H 0.6388 1.1609 0.7775 0.013 Uiso 1 1 calc R U H3B H 0.7014 1.1346 0.6372 0.013 Uiso 1 1 calc R U C4 C 0.4376(4) 0.9139(4) 0.6770(3) 0.0111(6) Uani 1 1 d . . H4A H 0.3972 0.8748 0.5891 0.013 Uiso 1 1 calc R U H4B H 0.3346 0.9011 0.7294 0.013 Uiso 1 1 calc R U N1 N 0.5825(3) 0.8316(3) 0.8624(2) 0.0075(5) Uani 1 1 d . . N2 N 0.4679(3) 0.6855(3) 1.0239(2) 0.0097(5) Uani 1 1 d . . H2 H 0.3905 0.6052 1.0723 0.012 Uiso 1 1 calc R U C21 C 0.4330(4) 0.6935(4) 0.9048(3) 0.0091(6) Uani 1 1 d . . H21 H 0.3207 0.6144 0.8572 0.011 Uiso 1 1 calc R U C41 C 0.6437(4) 0.8218(4) 1.0611(3) 0.0123(6) Uani 1 1 d . . H41 H 0.7031 0.8453 1.1424 0.015 Uiso 1 1 calc R U C51 C 0.7162(4) 0.9163(4) 0.9603(3) 0.0088(6) Uani 1 1 d . . H51 H 0.8352 1.0200 0.9572 0.011 Uiso 1 1 calc R U O1W O 0.9485(3) 0.5177(3) 0.36140(18) 0.0133(4) Uani 1 1 d D . H1W H 1.0664 0.5735 0.3720 0.020 Uiso 1 1 d DR U H2W H 0.9156 0.4063 0.3806 0.020 Uiso 1 1 d DR U O2W O 0.9764(3) 0.6453(3) 0.0969(2) 0.0380(6) Uani 1 1 d D . H3W H 1.0550 0.6026 0.1185 0.057 Uiso 1 1 d DR U H4W H 0.9410 0.6771 0.1613 0.057 Uiso 1 1 d DR 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 0.0065(2) 0.0060(2) 0.0066(2) 0.00054(16) 0.00130(16) 0.00212(15) P1 0.0049(4) 0.0053(4) 0.0065(4) 0.0000(3) 0.0006(3) 0.0013(3) P2 0.0068(4) 0.0042(4) 0.0062(4) 0.0005(3) 0.0010(3) 0.0019(3) O1 0.0062(10) 0.0041(10) 0.0096(11) 0.0000(8) 0.0014(8) -0.0010(8) O2 0.0063(10) 0.0076(10) 0.0086(11) -0.0002(8) -0.0002(8) 0.0026(8) O3 0.0074(11) 0.0061(10) 0.0115(12) 0.0028(8) 0.0005(8) -0.0005(8) O4 0.0062(10) 0.0068(10) 0.0072(11) -0.0007(8) 0.0024(8) -0.0003(8) O5 0.0070(10) 0.0071(10) 0.0082(11) 0.0009(8) 0.0015(8) 0.0026(8) O6 0.0089(10) 0.0057(10) 0.0078(11) -0.0005(8) 0.0026(8) 0.0025(8) O7 0.0066(10) 0.0065(10) 0.0030(9) 0.0010(8) 0.0000(8) 0.0015(8) C1 0.0047(14) 0.0061(14) 0.0057(14) 0.0011(11) -0.0002(11) 0.0016(11) C2 0.0062(14) 0.0064(14) 0.0049(14) 0.0013(11) 0.0013(11) 0.0029(11) C3 0.0143(16) 0.0103(15) 0.0117(16) 0.0018(12) 0.0028(13) 0.0086(12) C4 0.0087(16) 0.0164(16) 0.0113(15) -0.0001(13) 0.0016(13) 0.0081(12) N1 0.0086(12) 0.0071(12) 0.0074(12) 0.0013(10) 0.0020(10) 0.0037(10) N2 0.0126(13) 0.0063(12) 0.0087(13) 0.0009(10) 0.0048(10) 0.0022(10) C21 0.0115(15) 0.0091(15) 0.0083(16) -0.0012(12) 0.0038(12) 0.0054(12) C41 0.0138(17) 0.0131(16) 0.0103(15) -0.0040(12) -0.0024(13) 0.0066(13) C51 0.0063(14) 0.0096(15) 0.0084(14) -0.0025(12) 0.0000(11) 0.0015(12) O1W 0.0100(11) 0.0088(11) 0.0222(12) 0.0029(9) 0.0042(9) 0.0046(8) O2W 0.0345(16) 0.0411(16) 0.0376(16) 0.0030(13) 0.0052(13) 0.0147(12) 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' Co Co 0.3494 0.9721 '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' 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 O4 Co1 O1 92.69(8) 2_666 2_776 O4 Co1 O2 171.79(8) 2_666 . O1 Co1 O2 89.88(8) 2_776 . O4 Co1 O1W 92.10(8) 2_666 . O1 Co1 O1W 88.28(8) 2_776 . O2 Co1 O1W 95.77(8) . . O4 Co1 O6 91.34(8) 2_666 . O1 Co1 O6 175.96(8) 2_776 . O2 Co1 O6 86.17(8) . . O1W Co1 O6 91.27(8) . . O4 Co1 O7 89.38(8) 2_666 . O1 Co1 O7 100.45(8) 2_776 . O2 Co1 O7 82.48(8) . . O1W Co1 O7 171.08(7) . . O6 Co1 O7 79.89(7) . . O1 P1 O2 117.39(12) . . O1 P1 O3 105.77(12) . . O2 P1 O3 111.53(11) . . O1 P1 C1 114.02(12) . . O2 P1 C1 102.90(12) . . O3 P1 C1 104.66(12) . . O4 P2 O5 112.58(12) . . O4 P2 O6 112.76(11) . . O5 P2 O6 113.01(11) . . O4 P2 C1 108.18(12) . . O5 P2 C1 106.55(12) . . O6 P2 C1 102.98(11) . . P1 O1 Co1 135.86(12) . 2_776 P1 O2 Co1 116.03(11) . . P1 O3 H3 109.5 . . P2 O4 Co1 132.17(12) . 2_666 P2 O6 Co1 115.73(10) . . C1 O7 Co1 104.47(14) . . C1 O7 H7 105.7 . . Co1 O7 H7 98.0 . . O7 C1 C2 108.7(2) . . O7 C1 P2 107.62(17) . . C2 C1 P2 114.84(18) . . O7 C1 P1 102.47(17) . . C2 C1 P1 114.24(18) . . P2 C1 P1 108.10(13) . . N1 C2 C3 116.1(2) . . N1 C2 C4 114.1(2) . . C3 C2 C4 59.87(17) . . N1 C2 C1 115.5(2) . . C3 C2 C1 119.0(2) . . C4 C2 C1 120.9(2) . . C4 C3 C2 60.19(17) . . C4 C3 H3A 117.8 . . C2 C3 H3A 117.8 . . C4 C3 H3B 117.8 . . C2 C3 H3B 117.8 . . H3A C3 H3B 114.9 . . C3 C4 C2 59.94(18) . . C3 C4 H4A 117.8 . . C2 C4 H4A 117.8 . . C3 C4 H4B 117.8 . . C2 C4 H4B 117.8 . . H4A C4 H4B 114.9 . . C21 N1 C51 108.6(2) . . C21 N1 C2 124.4(2) . . C51 N1 C2 127.0(2) . . C21 N2 C41 109.6(2) . . C21 N2 H2 125.2 . . C41 N2 H2 125.2 . . N2 C21 N1 108.3(3) . . N2 C21 H21 125.8 . . N1 C21 H21 125.8 . . C51 C41 N2 107.1(3) . . C51 C41 H41 126.5 . . N2 C41 H41 126.5 . . C41 C51 N1 106.4(2) . . C41 C51 H51 126.8 . . N1 C51 H51 126.8 . . Co1 O1W H1W 112.5 . . Co1 O1W H2W 119.9 . . H1W O1W H2W 108.3 . . H3W O2W H4W 107.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 O4 2.023(2) 2_666 Co1 O1 2.071(2) 2_776 Co1 O2 2.081(2) . Co1 O1W 2.1161(19) . Co1 O6 2.183(2) . Co1 O7 2.1888(18) . P1 O1 1.498(2) . P1 O2 1.512(2) . P1 O3 1.579(2) . P1 C1 1.868(3) . P2 O4 1.517(2) . P2 O5 1.523(2) . P2 O6 1.539(2) . P2 C1 1.866(3) . O1 Co1 2.071(2) 2_776 O3 H3 0.8400 . O4 Co1 2.023(2) 2_666 O7 C1 1.447(3) . O7 H7 0.8397 . C1 C2 1.532(4) . C2 N1 1.456(3) . C2 C3 1.498(4) . C2 C4 1.502(4) . C3 C4 1.497(4) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 H4A 0.9900 . C4 H4B 0.9900 . N1 C21 1.336(3) . N1 C51 1.388(4) . N2 C21 1.315(4) . N2 C41 1.374(3) . N2 H2 0.8800 . C21 H21 0.9500 . C41 C51 1.353(4) . C41 H41 0.9500 . C51 H51 0.9500 . O1W H1W 0.8392 . O1W H2W 0.8392 . O2W H3W 0.8421 . O2W H4W 0.8420 . 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 O3 H3 O5 0.84 1.80 2.602(3) 158.6 . O7 H7 O6 0.84 1.87 2.703(3) 168.5 2_666 C3 H3A O5 0.99 2.60 3.350(4) 132.9 1_565 C4 H4B O3 0.99 2.60 3.566(4) 164.3 1_455 N2 H2 O5 0.88 1.82 2.682(3) 165.6 2_667 C21 H21 O2W 0.95 2.46 3.195(4) 134.5 2_666 C41 H41 O1 0.95 2.60 3.493(4) 157.7 2_777 C41 H41 O3 0.95 2.52 3.084(4) 118.2 2_777 C51 H51 O2W 0.95 2.52 3.374(4) 149.1 2_776 O1W H1W O6 0.84 2.23 2.950(3) 143.4 2_766 O1W H2W O2 0.84 2.05 2.806(3) 150.2 2_766 O2W H3W O5 0.84 2.39 3.227(3) 173.7 2_766 O2W H4W O1 0.84 2.30 3.075(3) 153.7 2_776 O2W H4W O1W 0.84 2.54 3.055(3) 120.4 . 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 O2 P1 O1 Co1 11.8(2) 2_776 O3 P1 O1 Co1 136.97(16) 2_776 C1 P1 O1 Co1 -108.58(18) 2_776 O1 P1 O2 Co1 -106.70(13) . O3 P1 O2 Co1 131.06(11) . C1 P1 O2 Co1 19.38(14) . O5 P2 O4 Co1 -152.34(13) 2_666 O6 P2 O4 Co1 -23.0(2) 2_666 C1 P2 O4 Co1 90.19(17) 2_666 O4 P2 O6 Co1 117.59(12) . O5 P2 O6 Co1 -113.31(12) . C1 P2 O6 Co1 1.24(14) . Co1 O7 C1 C2 178.47(16) . Co1 O7 C1 P2 -56.60(16) . Co1 O7 C1 P1 57.23(15) . O4 P2 C1 O7 -82.29(18) . O5 P2 C1 O7 156.43(15) . O6 P2 C1 O7 37.28(18) . O4 P2 C1 C2 38.9(2) . O5 P2 C1 C2 -82.4(2) . O6 P2 C1 C2 158.42(18) . O4 P2 C1 P1 167.70(12) . O5 P2 C1 P1 46.42(16) . O6 P2 C1 P1 -72.73(15) . O1 P1 C1 O7 76.46(18) . O2 P1 C1 O7 -51.76(17) . O3 P1 C1 O7 -168.44(14) . O1 P1 C1 C2 -40.9(2) . O2 P1 C1 C2 -169.09(18) . O3 P1 C1 C2 74.2(2) . O1 P1 C1 P2 -170.05(12) . O2 P1 C1 P2 61.73(15) . O3 P1 C1 P2 -54.96(15) . O7 C1 C2 N1 165.1(2) . P2 C1 C2 N1 44.6(3) . P1 C1 C2 N1 -81.2(2) . O7 C1 C2 C3 -49.5(3) . P2 C1 C2 C3 -170.1(2) . P1 C1 C2 C3 64.2(3) . O7 C1 C2 C4 20.8(3) . P2 C1 C2 C4 -99.8(3) . P1 C1 C2 C4 134.5(2) . N1 C2 C3 C4 -104.0(3) . C1 C2 C3 C4 110.9(3) . N1 C2 C4 C3 107.4(3) . C1 C2 C4 C3 -107.8(3) . C3 C2 N1 C21 120.3(3) . C4 C2 N1 C21 53.4(3) . C1 C2 N1 C21 -93.4(3) . C3 C2 N1 C51 -60.8(3) . C4 C2 N1 C51 -127.7(3) . C1 C2 N1 C51 85.5(3) . C41 N2 C21 N1 0.3(3) . C51 N1 C21 N2 -1.0(3) . C2 N1 C21 N2 178.0(2) . C21 N2 C41 C51 0.6(3) . N2 C41 C51 N1 -1.2(3) . C21 N1 C51 C41 1.4(3) . C2 N1 C51 C41 -177.7(2) .