#------------------------------------------------------------------------------ #$Date: 2019-10-08 06:42:39 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219150 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234444.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_7234444 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 N2 Ni O8 P2, (H2 O)' _chemical_formula_sum 'C7 H14 N2 Ni O9 P2' _chemical_formula_weight 390.85 _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 direct _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 91.03(3) _cell_angle_beta 93.26(3) _cell_angle_gamma 114.92(3) _cell_formula_units_Z 2 _cell_length_a 7.816(3) _cell_length_b 7.849(3) _cell_length_c 10.849(4) _cell_measurement_reflns_used 595 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.73 _cell_measurement_theta_min 2.85 _cell_volume 602.0(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 100(2) _diffrn_detector_area_resol_mean 10.3456 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.2248 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 5948 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.489 _diffrn_reflns_theta_min 2.865 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 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 greenish _exptl_crystal_density_diffrn 2.156 _exptl_crystal_description column _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.836 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.139 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.696 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 3636 _refine_ls_number_restraints 133 _refine_ls_restrained_S_all 0.693 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0421 _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^)+(0.0128P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.0603 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1815 _reflns_number_total 3636 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra05673d2.cif _cod_data_source_block tr21114ab _cod_database_code 7234444 _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 0.801 _shelx_estimated_absorpt_t_max 0.981 _shelx_res_file ; tr21114ab.res created by SHELXL-2014/7 TITL tr21114_a.res in P-1 CELL 0.71073 7.816 7.849 10.849 91.03 93.26 114.92 ZERR 2 0.003 0.003 0.004 0.03 0.03 0.03 LATT 1 SFAC C H N Ni O P UNIT 14 28 4 2 18 4 ISOR 0.002 0.004 L.S. 10 PLAN 5 BOND $H HTAB temp -173 size 0.12 0.01 0.01 CONF fmap 2 acta OMIT 0 51 OMIT 2 3 5 EQIV $1 -x+1, -y+1, -z+1 EQIV $2 x, y+1, z EQIV $3 x-1, y, z EQIV $4 -x+1, -y+1, -z+2 EQIV $5 -x+2, -y+2, -z+2 EQIV $6 -x+2, -y+2, -z+1 EQIV $7 -x+2, -y+1, -z+1 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 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 0.012800 BASF 0.49006 FVAR 1.21215 NI1 4 0.811980 0.674203 0.434030 11.00000 0.00918 0.00880 = 0.00937 0.00005 0.00133 0.00405 P1 6 0.964482 0.903023 0.675392 11.00000 0.00592 0.00669 = 0.00536 0.00113 0.00087 0.00073 O1 5 1.047983 1.114170 0.680441 11.00000 0.00723 0.00322 = 0.00356 -0.00022 0.00240 0.00085 O2 5 1.020185 0.805450 0.573780 11.00000 0.00452 0.00770 = 0.00998 -0.00166 -0.00072 0.00495 O3 5 1.013767 0.847751 0.807368 11.00000 0.00983 0.00724 = 0.00840 -0.00105 -0.00160 -0.00055 AFIX 147 H3 2 0.942555 0.734589 0.817774 11.00000 -1.50000 AFIX 0 P2 6 0.620761 0.529569 0.680181 11.00000 0.00919 0.00347 = 0.00781 -0.00025 -0.00062 0.00142 O4 5 0.410563 0.442407 0.693400 11.00000 0.00722 0.00777 = 0.00845 0.00062 -0.00022 0.00133 O5 5 0.734421 0.517548 0.796412 11.00000 0.00797 0.00199 = 0.00885 0.00172 -0.00309 -0.00155 O6 5 0.677918 0.460528 0.561858 11.00000 0.00776 0.00285 = 0.00760 -0.00045 0.00485 0.00038 O7 5 0.664202 0.806434 0.526143 11.00000 0.00661 0.00754 = 0.00846 -0.00063 0.00056 0.00403 AFIX 3 H7 2 0.550660 0.732116 0.508147 11.00000 -1.50000 AFIX 0 C1 1 0.700401 0.786132 0.656472 11.00000 0.00518 0.00809 = 0.00362 -0.00048 0.00152 0.00086 C2 1 0.601989 0.881618 0.733041 11.00000 0.00578 0.00728 = 0.00864 0.00161 -0.00113 0.00432 C3 1 0.633252 1.076690 0.705416 11.00000 0.01171 0.00867 = 0.01049 -0.00058 -0.00027 0.00587 AFIX 23 H3A 2 0.710350 1.135124 0.635518 11.00000 -1.20000 H3B 2 0.647204 1.164474 0.775929 11.00000 -1.20000 AFIX 0 C4 1 0.440633 0.915309 0.675685 11.00000 0.01119 0.01472 = 0.01574 -0.00095 0.00070 0.00903 AFIX 23 H4A 2 0.337330 0.904340 0.728249 11.00000 -1.20000 H4B 2 0.400515 0.874972 0.587752 11.00000 -1.20000 AFIX 0 N1 3 0.585357 0.834225 0.860719 11.00000 0.00769 0.00555 = 0.00472 -0.00170 0.00362 0.00243 N2 3 0.467870 0.687278 1.024084 11.00000 0.01274 0.00702 = 0.00769 0.00398 0.00533 0.00432 AFIX 43 H2 2 0.389935 0.606599 1.072754 11.00000 -1.20000 AFIX 0 C21 1 0.433435 0.696465 0.905254 11.00000 0.00904 0.00902 = 0.00999 -0.00394 0.00075 0.00402 AFIX 43 H21 2 0.319803 0.618610 0.858219 11.00000 -1.20000 AFIX 0 C41 1 0.646356 0.824650 1.060988 11.00000 0.00803 0.00602 = 0.00354 -0.00291 -0.00122 0.00106 AFIX 43 H41 2 0.706442 0.849416 1.142093 11.00000 -1.20000 AFIX 0 C51 1 0.717015 0.915340 0.959510 11.00000 0.00840 0.01118 = 0.01507 -0.00121 0.00284 0.00676 AFIX 43 H51 2 0.837330 1.018110 0.955945 11.00000 -1.20000 AFIX 0 O1W 5 0.946711 0.522069 0.363108 11.00000 0.01003 0.00876 = 0.01932 -0.00072 0.00741 0.00371 AFIX 3 H1W 2 1.065046 0.573421 0.361010 11.00000 -1.50000 H2W 2 0.913334 0.406406 0.371452 11.00000 -1.50000 AFIX 0 O2W 5 0.973781 0.646318 0.096599 11.00000 0.05088 0.04458 = 0.05252 0.00741 0.00627 0.01771 AFIX 3 H3W 2 1.016338 0.565950 0.110535 11.00000 -1.50000 H4W 2 0.964035 0.692455 0.164917 11.00000 -1.50000 AFIX 0 HKLF 5 REM tr21114_a.res in P-1 REM R1 = 0.0421 for 1815 Fo > 4sig(Fo) and 0.1023 for all 3636 data REM 192 parameters refined using 133 restraints END WGHT 0.0128 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 0.836, deepest hole -0.750, 1-sigma level 0.139 Q1 1 0.6806 0.5374 0.5794 11.00000 0.05 0.58 Q2 1 0.3641 0.3006 0.7049 11.00000 0.05 0.50 Q3 1 0.8372 0.8403 0.6183 11.00000 0.05 0.49 Q4 1 0.2559 0.8864 0.5524 11.00000 0.05 0.48 Q5 1 0.4877 0.6855 0.9567 11.00000 0.05 0.48 ; _shelx_res_checksum 25435 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 Ni1 Ni 0.81198(12) 0.67420(12) 0.43403(8) 0.0090(2) Uani 1 1 d . U P1 P 0.9645(2) 0.9030(2) 0.67539(16) 0.0066(4) Uani 1 1 d . U O1 O 1.0480(5) 1.1142(5) 0.6804(3) 0.0051(9) Uani 1 1 d . U O2 O 1.0202(5) 0.8055(4) 0.5738(3) 0.0067(10) Uani 1 1 d . U O3 O 1.0138(5) 0.8478(5) 0.8074(3) 0.0100(10) Uani 1 1 d . U H3 H 0.9426 0.7346 0.8178 0.015 Uiso 1 1 calc R U P2 P 0.6208(2) 0.5296(2) 0.68018(15) 0.0073(4) Uani 1 1 d . U O4 O 0.4106(5) 0.4424(5) 0.6934(4) 0.0085(10) Uani 1 1 d . U O5 O 0.7344(5) 0.5175(5) 0.7964(3) 0.0077(10) Uani 1 1 d . U O6 O 0.6779(5) 0.4605(4) 0.5619(3) 0.0065(10) Uani 1 1 d . U O7 O 0.6642(5) 0.8064(5) 0.5261(3) 0.0072(10) Uani 1 1 d D U H7 H 0.5507 0.7321 0.5081 0.011 Uiso 1 1 d DR U C1 C 0.7004(7) 0.7861(7) 0.6565(5) 0.0063(13) Uani 1 1 d . U C2 C 0.6020(7) 0.8816(7) 0.7330(5) 0.0068(14) Uani 1 1 d . U C3 C 0.6333(8) 1.0767(8) 0.7054(5) 0.0098(14) Uani 1 1 d . U H3A H 0.7104 1.1351 0.6355 0.012 Uiso 1 1 calc R U H3B H 0.6472 1.1645 0.7759 0.012 Uiso 1 1 calc R U C4 C 0.4406(8) 0.9153(8) 0.6757(5) 0.0127(14) Uani 1 1 d . U H4A H 0.3373 0.9043 0.7282 0.015 Uiso 1 1 calc R U H4B H 0.4005 0.8750 0.5878 0.015 Uiso 1 1 calc R U N1 N 0.5854(6) 0.8342(6) 0.8607(4) 0.0060(11) Uani 1 1 d . U N2 N 0.4679(6) 0.6873(6) 1.0241(4) 0.0089(12) Uani 1 1 d . U H2 H 0.3899 0.6066 1.0728 0.011 Uiso 1 1 calc R U C21 C 0.4334(8) 0.6965(7) 0.9053(6) 0.0093(15) Uani 1 1 d . U H21 H 0.3198 0.6186 0.8582 0.011 Uiso 1 1 calc R U C41 C 0.6464(7) 0.8247(7) 1.0610(5) 0.0066(13) Uani 1 1 d . U H41 H 0.7064 0.8494 1.1421 0.008 Uiso 1 1 calc R U C51 C 0.7170(8) 0.9153(8) 0.9595(5) 0.0106(14) Uani 1 1 d . U H51 H 0.8373 1.0181 0.9559 0.013 Uiso 1 1 calc R U O1W O 0.9467(5) 0.5221(5) 0.3631(3) 0.0125(10) Uani 1 1 d D U H1W H 1.0650 0.5734 0.3610 0.019 Uiso 1 1 d DR U H2W H 0.9133 0.4064 0.3715 0.019 Uiso 1 1 d DR U O2W O 0.9738(6) 0.6463(6) 0.0966(4) 0.0500(14) Uani 1 1 d D U H3W H 1.0163 0.5659 0.1105 0.075 Uiso 1 1 d DR U H4W H 0.9640 0.6925 0.1649 0.075 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 Ni1 0.0092(5) 0.0088(5) 0.0094(5) 0.0000(4) 0.0013(4) 0.0041(4) P1 0.0059(9) 0.0067(9) 0.0054(10) 0.0011(7) 0.0009(7) 0.0007(7) O1 0.0072(18) 0.0032(17) 0.0036(19) -0.0002(14) 0.0024(15) 0.0009(14) O2 0.0045(18) 0.0077(18) 0.010(2) -0.0017(15) -0.0007(15) 0.0049(15) O3 0.010(2) 0.007(2) 0.008(2) -0.0010(17) -0.0016(18) -0.0005(19) P2 0.0092(9) 0.0035(8) 0.0078(10) -0.0003(7) -0.0006(7) 0.0014(7) O4 0.0072(18) 0.0078(18) 0.008(2) 0.0006(15) -0.0002(15) 0.0013(15) O5 0.008(2) 0.002(2) 0.009(2) 0.0017(16) -0.0031(17) -0.0016(18) O6 0.0078(18) 0.0028(17) 0.0076(19) -0.0004(15) 0.0049(15) 0.0004(15) O7 0.0066(18) 0.0075(17) 0.0085(19) -0.0006(15) 0.0006(15) 0.0040(15) C1 0.005(2) 0.008(2) 0.004(2) -0.0005(18) 0.0015(18) 0.0009(18) C2 0.006(2) 0.007(2) 0.009(2) 0.0016(18) -0.0011(18) 0.0043(19) C3 0.012(2) 0.009(2) 0.010(2) -0.0006(19) -0.0003(19) 0.0059(19) C4 0.011(2) 0.015(2) 0.016(2) -0.0010(19) 0.0007(19) 0.0090(19) N1 0.008(2) 0.006(2) 0.005(2) -0.0017(17) 0.0036(17) 0.0024(17) N2 0.013(2) 0.007(2) 0.008(2) 0.0040(17) 0.0053(17) 0.0043(17) C21 0.009(2) 0.009(2) 0.010(3) -0.0039(19) 0.0007(19) 0.0040(19) C41 0.008(2) 0.006(2) 0.004(2) -0.0029(18) -0.0012(19) 0.0011(19) C51 0.008(2) 0.011(2) 0.015(2) -0.0012(19) 0.0028(19) 0.0068(19) O1W 0.010(2) 0.009(2) 0.019(2) -0.0007(18) 0.0074(18) 0.0037(17) O2W 0.051(3) 0.045(3) 0.053(3) 0.007(2) 0.006(2) 0.018(2) 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' Ni Ni 0.3393 1.1124 '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 Ni1 O1 91.15(15) 2_666 2_776 O4 Ni1 O1W 92.46(15) 2_666 . O1 Ni1 O1W 89.23(15) 2_776 . O4 Ni1 O2 173.47(16) 2_666 . O1 Ni1 O2 90.09(16) 2_776 . O1W Ni1 O2 93.97(15) . . O4 Ni1 O7 89.43(15) 2_666 . O1 Ni1 O7 97.95(14) 2_776 . O1W Ni1 O7 172.54(16) . . O2 Ni1 O7 84.05(14) . . O4 Ni1 O6 92.07(15) 2_666 . O1 Ni1 O6 176.76(17) 2_776 . O1W Ni1 O6 90.95(14) . . O2 Ni1 O6 86.68(14) . . O7 Ni1 O6 81.77(14) . . O1 P1 O2 117.9(2) . . O1 P1 O3 105.6(2) . . O2 P1 O3 111.5(2) . . O1 P1 C1 114.5(2) . . O2 P1 C1 102.5(2) . . O3 P1 C1 104.2(2) . . P1 O1 Ni1 137.2(2) . 2_776 P1 O2 Ni1 114.8(2) . . P1 O3 H3 109.5 . . O4 P2 O5 112.9(2) . . O4 P2 O6 113.6(2) . . O5 P2 O6 112.6(2) . . O4 P2 C1 108.7(2) . . O5 P2 C1 105.6(2) . . O6 P2 C1 102.5(2) . . P2 O4 Ni1 131.4(2) . 2_666 P2 O6 Ni1 115.00(18) . . C1 O7 Ni1 104.5(3) . . C1 O7 H7 106.0 . . Ni1 O7 H7 102.3 . . O7 C1 C2 109.0(4) . . O7 C1 P2 107.3(3) . . C2 C1 P2 114.7(4) . . O7 C1 P1 102.0(3) . . C2 C1 P1 114.4(4) . . P2 C1 P1 108.5(3) . . N1 C2 C3 116.6(4) . . N1 C2 C4 114.5(4) . . C3 C2 C4 61.1(3) . . N1 C2 C1 115.2(4) . . C3 C2 C1 118.3(5) . . C4 C2 C1 120.5(5) . . C2 C3 C4 59.9(3) . . C2 C3 H3A 117.8 . . C4 C3 H3A 117.8 . . C2 C3 H3B 117.8 . . C4 C3 H3B 117.8 . . H3A C3 H3B 114.9 . . C2 C4 C3 59.0(3) . . C2 C4 H4A 117.9 . . C3 C4 H4A 117.9 . . C2 C4 H4B 117.9 . . C3 C4 H4B 117.9 . . H4A C4 H4B 115.0 . . C21 N1 C51 107.0(5) . . C21 N1 C2 124.8(5) . . C51 N1 C2 128.1(5) . . C21 N2 C41 109.3(5) . . C21 N2 H2 125.3 . . C41 N2 H2 125.3 . . N2 C21 N1 108.9(5) . . N2 C21 H21 125.5 . . N1 C21 H21 125.5 . . C51 C41 N2 106.2(5) . . C51 C41 H41 126.9 . . N2 C41 H41 126.9 . . C41 C51 N1 108.5(5) . . C41 C51 H51 125.8 . . N1 C51 H51 125.8 . . Ni1 O1W H1W 119.1 . . Ni1 O1W H2W 124.6 . . H1W O1W H2W 107.9 . . H3W O2W H4W 108.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 O4 2.028(4) 2_666 Ni1 O1 2.048(4) 2_776 Ni1 O1W 2.060(3) . Ni1 O2 2.064(4) . Ni1 O7 2.125(3) . Ni1 O6 2.145(4) . P1 O1 1.502(4) . P1 O2 1.515(4) . P1 O3 1.577(4) . P1 C1 1.869(5) . O1 Ni1 2.048(4) 2_776 O3 H3 0.8400 . P2 O4 1.507(4) . P2 O5 1.528(4) . P2 O6 1.544(4) . P2 C1 1.868(5) . O4 Ni1 2.028(4) 2_666 O7 C1 1.451(6) . O7 H7 0.8402 . C1 C2 1.543(7) . C2 N1 1.440(6) . C2 C3 1.484(7) . C2 C4 1.498(7) . C3 C4 1.516(7) . C3 H3A 0.9900 . C3 H3B 0.9900 . C4 H4A 0.9900 . C4 H4B 0.9900 . N1 C21 1.347(6) . N1 C51 1.382(6) . N2 C21 1.311(7) . N2 C41 1.387(6) . N2 H2 0.8800 . C21 H21 0.9500 . C41 C51 1.338(7) . C41 H41 0.9500 . C51 H51 0.9500 . O1W H1W 0.8408 . O1W H2W 0.8405 . O2W H3W 0.8402 . O2W H4W 0.8404 . 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 1.79 2.586(5) 157.2 . O7 H7 O6 0.84 1.89 2.714(5) 165.5 2_666 C3 H3B O5 0.99 2.56 3.325(6) 133.8 1_565 C4 H4A O3 0.99 2.58 3.540(7) 164.1 1_455 N2 H2 O5 0.88 1.82 2.683(6) 165.7 2_667 C21 H21 O2W 0.95 2.44 3.185(7) 134.7 2_666 C41 H41 O1 0.95 2.56 3.468(6) 159.3 2_777 C41 H41 O3 0.95 2.48 3.064(6) 119.4 2_777 C51 H51 O2W 0.95 2.51 3.359(7) 148.4 2_776 O1W H1W O6 0.84 2.25 2.945(5) 139.8 2_766 O1W H2W O2 0.84 2.03 2.784(5) 149.0 2_766 O2W H3W O5 0.84 2.47 3.229(6) 150.1 2_766 O2W H4W O1 0.84 2.27 3.093(6) 164.6 2_776 O2W H4W O1W 0.84 2.53 3.058(6) 121.6 . 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 Ni1 14.9(5) 2_776 O3 P1 O1 Ni1 140.2(3) 2_776 C1 P1 O1 Ni1 -105.8(3) 2_776 O1 P1 O2 Ni1 -106.8(3) . O3 P1 O2 Ni1 130.9(2) . C1 P1 O2 Ni1 20.0(3) . O5 P2 O4 Ni1 -153.5(2) 2_666 O6 P2 O4 Ni1 -23.7(4) 2_666 C1 P2 O4 Ni1 89.6(3) 2_666 O4 P2 O6 Ni1 117.0(2) . O5 P2 O6 Ni1 -113.1(2) . C1 P2 O6 Ni1 -0.1(3) . Ni1 O7 C1 C2 178.9(3) . Ni1 O7 C1 P2 -56.3(3) . Ni1 O7 C1 P1 57.6(3) . O4 P2 C1 O7 -83.0(3) . O5 P2 C1 O7 155.6(3) . O6 P2 C1 O7 37.5(4) . O4 P2 C1 C2 38.3(4) . O5 P2 C1 C2 -83.2(4) . O6 P2 C1 C2 158.8(4) . O4 P2 C1 P1 167.5(2) . O5 P2 C1 P1 46.1(3) . O6 P2 C1 P1 -72.0(3) . O1 P1 C1 O7 76.9(3) . O2 P1 C1 O7 -52.0(3) . O3 P1 C1 O7 -168.3(3) . O1 P1 C1 C2 -40.6(5) . O2 P1 C1 C2 -169.5(4) . O3 P1 C1 C2 74.2(4) . O1 P1 C1 P2 -170.1(2) . O2 P1 C1 P2 61.1(3) . O3 P1 C1 P2 -55.2(3) . O7 C1 C2 N1 165.3(4) . P2 C1 C2 N1 45.1(6) . P1 C1 C2 N1 -81.2(5) . O7 C1 C2 C3 -50.0(6) . P2 C1 C2 C3 -170.3(4) . P1 C1 C2 C3 63.4(6) . O7 C1 C2 C4 21.3(7) . P2 C1 C2 C4 -99.0(5) . P1 C1 C2 C4 134.7(4) . N1 C2 C3 C4 -104.7(5) . C1 C2 C3 C4 111.1(5) . N1 C2 C4 C3 108.0(5) . C1 C2 C4 C3 -107.7(6) . C3 C2 N1 C21 120.6(5) . C4 C2 N1 C21 52.1(7) . C1 C2 N1 C21 -94.1(6) . C3 C2 N1 C51 -60.1(7) . C4 C2 N1 C51 -128.7(5) . C1 C2 N1 C51 85.1(6) . C41 N2 C21 N1 1.1(6) . C51 N1 C21 N2 -1.5(6) . C2 N1 C21 N2 177.9(4) . C21 N2 C41 C51 -0.2(6) . N2 C41 C51 N1 -0.7(6) . C21 N1 C51 C41 1.3(6) . C2 N1 C51 C41 -178.0(5) .