#------------------------------------------------------------------------------ #$Date: 2019-10-08 06:42:58 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219151 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234446.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_7234446 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 N2 Ni3 O20 P4, 4(H2 O)' _chemical_formula_sum 'C12 H44 N2 Ni3 O24 P4' _chemical_formula_weight 900.50 _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_block_doi 10.5517/ccdc.csd.cc22gnz6 _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 114.954(5) _cell_angle_beta 97.790(5) _cell_angle_gamma 90.883(6) _cell_formula_units_Z 1 _cell_length_a 9.056(3) _cell_length_b 9.430(3) _cell_length_c 9.605(3) _cell_measurement_reflns_used 695 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.94 _cell_measurement_theta_min 2.37 _cell_volume 734.4(4) _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 0.983 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0845 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 7996 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 2.277 _exptl_absorpt_coefficient_mu 2.224 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_correction_T_min 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.036 _exptl_crystal_description block _exptl_crystal_F_000 466 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.856 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.140 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 205 _refine_ls_number_reflns 2819 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0561 _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^)+(0.0530P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1141 _refine_ls_wR_factor_ref 0.1226 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2134 _reflns_number_total 2819 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra05722f2.cif _cod_data_source_block Ni-1 _cod_database_code 7234446 _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 0.776 _shelx_estimated_absorpt_t_max 0.842 _shelx_res_file ; TITL Ni in P-1 Ni-1.res created by SHELXL-2018/3 at 14:25:50 on 05-Jun-2019 CELL 0.71073 9.0558 9.4303 9.6053 114.9543 97.7905 90.8825 ZERR 1.00 0.0025 0.0026 0.0026 0.0054 0.0054 0.0061 LATT 1 SFAC C H N O P Ni UNIT 12 44 2 24 4 3 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_$7 HTAB O3W O4W_$8 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 O5W_$5 HTAB C5 O4W HTAB C5 O7_$4 HTAB C4 O4_$3 HTAB C3 O7 HTAB C2 O2 HTAB O5W O3_$3 HTAB O5W O2_$3 HTAB O5W O2_$5 HTAB O4W O7_$4 HTAB O4W O7_$9 HTAB O3W O5W_$7 HTAB O3W O4W_$8 HTAB O3W O1W_$6 HTAB O2W O5W_$10 EQIV $10 x+1, y+1, z 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 O5W_$5 HTAB C5 O4W HTAB C5 O7_$4 HTAB C4 O4_$3 HTAB C3 O7 HTAB C2 O2 HTAB O5W O3_$3 HTAB O5W O2_$3 HTAB O5W O2_$5 HTAB O4W O7_$4 HTAB O4W O7_$9 EQIV $9 x, y-1, z HTAB O3W O4W_$8 EQIV $8 x, y+1, z HTAB O3W O5W_$7 EQIV $7 -x+1, -y+2, -z+2 HTAB O2W O6_$6 HTAB O1W O6 HTAB O1W O4 HTAB O1W O3W_$6 EQIV $6 -x+2, -y+2, -z+1 HTAB N1 O5_$4 HTAB N1 O5W HTAB C6 O3 HTAB C5 O5W_$5 EQIV $5 -x+1, -y+1, -z+2 HTAB C5 O4W HTAB C5 O7_$4 EQIV $4 -x+1, -y+1, -z+1 HTAB C4 O4_$3 EQIV $3 x-1, y, z HTAB C3 O7 HTAB C2 O2 HTAB CONF size 0.12 0.10 0.08 HTAB C2 O2 HTAB C3 O7 HTAB C4 O4_$3 HTAB C5 O7_$4 HTAB C5 O4W HTAB C5 O5W_$5 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 O5W_$7 HTAB O3W O4W_$8 HTAB O4W O7_$9 HTAB O4W O7_$4 HTAB O5W O2_$5 HTAB O5W O2_$3 HTAB O5W O3_$3 WGHT 0.053000 FVAR 0.14089 NI1 6 1.000000 0.500000 0.500000 10.50000 0.01513 0.01206 = 0.01247 0.00200 0.00180 0.00339 NI2 6 0.967572 1.057773 0.787547 11.00000 0.01929 0.01188 = 0.01140 0.00388 0.00094 0.00019 P1 5 0.967678 0.758831 0.841975 11.00000 0.01113 0.01137 = 0.01044 0.00393 0.00054 0.00212 P2 5 0.763890 0.769072 0.568849 11.00000 0.01541 0.01179 = 0.01019 0.00355 -0.00061 0.00253 C1 1 0.780320 0.806411 0.774877 11.00000 0.01214 0.00761 = 0.01259 0.00256 0.00129 0.00484 C2 1 0.654455 0.732363 0.820960 11.00000 0.01426 0.01705 = 0.01262 0.00677 0.00053 0.00181 AFIX 13 H2 2 0.682208 0.761011 0.932258 11.00000 -1.20000 AFIX 0 C3 1 0.502253 0.794306 0.801951 11.00000 0.01856 0.01475 = 0.03569 0.01016 0.00178 0.00315 AFIX 23 H3A 2 0.511980 0.908102 0.852370 11.00000 -1.20000 H3B 2 0.465592 0.761310 0.692355 11.00000 -1.20000 AFIX 0 C4 1 0.392360 0.733534 0.872536 11.00000 0.01387 0.03250 = 0.03835 0.01143 0.00581 0.00289 AFIX 23 H4A 2 0.425140 0.773348 0.983660 11.00000 -1.20000 H4B 2 0.295142 0.770734 0.856305 11.00000 -1.20000 AFIX 0 C5 1 0.526857 0.494407 0.810965 11.00000 0.02336 0.01693 = 0.02849 0.01080 0.00374 -0.00240 AFIX 23 H5A 2 0.513432 0.380815 0.757457 11.00000 -1.20000 H5B 2 0.566464 0.522920 0.919144 11.00000 -1.20000 AFIX 0 C6 1 0.637163 0.553441 0.740327 11.00000 0.01363 0.01714 = 0.02197 0.00528 0.00289 0.00031 AFIX 23 H6A 2 0.602263 0.518286 0.630086 11.00000 -1.20000 H6B 2 0.733041 0.512114 0.752543 11.00000 -1.20000 AFIX 0 N1 3 0.379796 0.559689 0.801334 11.00000 0.01836 0.03335 = 0.01429 0.00894 -0.00273 -0.00776 AFIX 23 H1A 2 0.338532 0.523883 0.701967 11.00000 -1.20000 H1B 2 0.319669 0.526403 0.849304 11.00000 -1.20000 AFIX 0 O1 4 0.786417 0.976702 0.857774 11.00000 0.01112 0.00826 = 0.01581 0.00186 0.00663 0.00390 AFIX 3 H1C 2 0.729407 1.031022 0.920324 11.00000 -1.20000 AFIX 0 O2 4 0.961910 0.767611 1.002387 11.00000 0.01789 0.01148 = 0.01065 0.00168 -0.00192 -0.00105 O3 4 1.004987 0.597218 0.735277 11.00000 0.01618 0.01041 = 0.01175 0.00154 0.00050 0.00222 O4 4 1.071903 0.890970 0.847132 11.00000 0.01246 0.01781 = 0.02026 0.00988 0.00225 0.00451 O5 4 0.802535 0.601331 0.478238 11.00000 0.01276 0.01359 = 0.01456 0.00267 -0.00091 0.00278 O6 4 0.884579 0.888711 0.574726 11.00000 0.02712 0.01334 = 0.00661 0.00017 0.00004 -0.00221 O7 4 0.610134 0.798519 0.513727 11.00000 0.02038 0.02268 = 0.02072 0.00645 -0.00016 0.00688 O1W 4 1.131277 0.693077 0.518157 11.00000 0.03013 0.01755 = 0.01993 0.00170 0.00939 0.00259 AFIX 3 H1WB 2 1.108498 0.707227 0.437127 11.00000 -1.50000 H1WA 2 1.114737 0.773167 0.595947 11.00000 -1.50000 AFIX 0 O2W 4 1.148512 1.108011 0.704856 11.00000 0.02981 0.05049 = 0.02499 0.02414 0.00259 -0.00222 AFIX 3 H2WA 2 1.216983 1.049700 0.710766 11.00000 -1.50000 H2WB 2 1.122712 1.091691 0.611326 11.00000 -1.50000 AFIX 0 O3W 4 0.836265 1.225317 0.749390 11.00000 0.04269 0.02147 = 0.02192 0.00948 -0.00497 0.00782 AFIX 3 H3WB 2 0.760235 1.179497 0.682081 11.00000 -1.50000 H3WA 2 0.808015 1.286057 0.833071 11.00000 -1.50000 AFIX 0 O4W 4 0.533416 0.106590 0.692807 11.00000 0.11861 0.03962 = 0.03968 0.00933 -0.02272 0.03048 AFIX 3 H4WA 2 0.547226 0.005040 0.644197 11.00000 -1.20000 H4WB 2 0.460876 0.136490 0.640077 11.00000 -1.20000 AFIX 0 O5W 4 0.159902 0.491156 0.952727 11.00000 0.01936 0.03350 = 0.04209 0.02625 0.00064 -0.00007 AFIX 3 H5WA 2 0.130392 0.403316 0.957937 11.00000 -1.20000 H5WB 2 0.095082 0.514296 0.887687 11.00000 -1.20000 AFIX 0 HKLF 4 REM Ni in P-1 REM wR2 = 0.1226, GooF = S = 1.001, Restrained GooF = 1.001 for all data REM R1 = 0.0561 for 2134 Fo > 4sig(Fo) and 0.0767 for all 2819 data REM 205 parameters refined using 0 restraints END WGHT 0.0525 0.0000 REM Instructions for potential hydrogen bonds HTAB C2 O2 HTAB C3 O7 HTAB C4 O4_$3 HTAB C5 O7_$4 HTAB C5 O4W HTAB C5 O5W_$5 HTAB C6 O3 HTAB N1 O5_$4 HTAB N1 O5W HTAB O1W O3W_$6 HTAB O1W O4 HTAB O1W O6 HTAB O2W O6_$6 HTAB O3W O4W_$8 HTAB O3W O5W_$7 HTAB O4W O7_$9 HTAB O4W O7_$4 HTAB O5W O2_$5 HTAB O5W O2_$3 HTAB O5W O3_$3 REM Highest difference peak 0.856, deepest hole -0.694, 1-sigma level 0.140 Q1 1 1.0367 1.1391 0.7771 11.00000 0.05 0.86 Q2 1 0.8662 0.7805 0.7997 11.00000 0.05 0.71 Q3 1 0.9181 0.9946 0.8425 11.00000 0.05 0.70 Q4 1 1.0628 0.5804 0.4780 11.00000 0.05 0.69 Q5 1 0.8835 0.5283 0.4918 11.00000 0.05 0.67 ; _shelx_res_checksum 8333 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 Ni1 Ni 1.000000 0.500000 0.500000 0.0144(3) Uani 1 2 d S . P Ni2 Ni 0.96757(8) 1.05777(9) 0.78755(8) 0.0147(2) Uani 1 1 d . . . P1 P 0.96768(15) 0.75883(17) 0.84197(15) 0.0113(3) Uani 1 1 d . . . P2 P 0.76389(16) 0.76907(18) 0.56885(16) 0.0131(3) Uani 1 1 d . . . C1 C 0.7803(6) 0.8064(6) 0.7749(6) 0.0114(11) Uani 1 1 d . . . C2 C 0.6545(6) 0.7324(7) 0.8210(6) 0.0146(12) Uani 1 1 d . . . H2 H 0.682208 0.761011 0.932258 0.018 Uiso 1 1 calc R U . C3 C 0.5023(6) 0.7943(7) 0.8020(7) 0.0235(14) Uani 1 1 d . . . H3A H 0.511980 0.908102 0.852370 0.028 Uiso 1 1 calc R U . H3B H 0.465592 0.761310 0.692355 0.028 Uiso 1 1 calc R U . C4 C 0.3924(7) 0.7335(8) 0.8725(8) 0.0294(16) Uani 1 1 d . . . H4A H 0.425140 0.773348 0.983660 0.035 Uiso 1 1 calc R U . H4B H 0.295142 0.770734 0.856305 0.035 Uiso 1 1 calc R U . C5 C 0.5269(6) 0.4944(7) 0.8110(7) 0.0226(14) Uani 1 1 d . . . H5A H 0.513432 0.380815 0.757457 0.027 Uiso 1 1 calc R U . H5B H 0.566464 0.522920 0.919144 0.027 Uiso 1 1 calc R U . C6 C 0.6372(6) 0.5534(7) 0.7403(7) 0.0187(13) Uani 1 1 d . . . H6A H 0.602263 0.518286 0.630086 0.022 Uiso 1 1 calc R U . H6B H 0.733041 0.512114 0.752543 0.022 Uiso 1 1 calc R U . N1 N 0.3798(5) 0.5597(6) 0.8013(5) 0.0231(12) Uani 1 1 d . . . H1A H 0.338532 0.523883 0.701967 0.028 Uiso 1 1 calc R U . H1B H 0.319669 0.526403 0.849304 0.028 Uiso 1 1 calc R U . O1 O 0.7864(4) 0.9767(4) 0.8578(4) 0.0124(8) Uani 1 1 d . . . H1C H 0.729407 1.031022 0.920324 0.015 Uiso 1 1 d R U . O2 O 0.9619(4) 0.7676(4) 1.0024(4) 0.0148(8) Uani 1 1 d . . . O3 O 1.0050(4) 0.5972(4) 0.7353(4) 0.0141(8) Uani 1 1 d . . . O4 O 1.0719(4) 0.8910(4) 0.8471(4) 0.0162(9) Uani 1 1 d . . . O5 O 0.8025(4) 0.6013(4) 0.4782(4) 0.0151(9) Uani 1 1 d . . . O6 O 0.8846(4) 0.8887(4) 0.5747(4) 0.0174(9) Uani 1 1 d . . . O7 O 0.6101(4) 0.7985(5) 0.5137(4) 0.0225(10) Uani 1 1 d . . . O1W O 1.1313(4) 0.6931(5) 0.5182(4) 0.0242(10) Uani 1 1 d . . . H1WB H 1.108498 0.707227 0.437127 0.036 Uiso 1 1 d R U . H1WA H 1.114737 0.773167 0.595947 0.036 Uiso 1 1 d R U . O2W O 1.1485(4) 1.1080(6) 0.7049(5) 0.0326(11) Uani 1 1 d . . . H2WA H 1.216983 1.049700 0.710766 0.049 Uiso 1 1 d R U . H2WB H 1.122712 1.091691 0.611326 0.049 Uiso 1 1 d R U . O3W O 0.8363(5) 1.2253(5) 0.7494(5) 0.0296(11) Uani 1 1 d . . . H3WB H 0.760235 1.179497 0.682081 0.044 Uiso 1 1 d R U . H3WA H 0.808015 1.286057 0.833071 0.044 Uiso 1 1 d R U . O4W O 0.5334(7) 0.1066(6) 0.6928(6) 0.072(2) Uani 1 1 d . . . H4WA H 0.547226 0.005040 0.644197 0.086 Uiso 1 1 d R U . H4WB H 0.460876 0.136490 0.640077 0.086 Uiso 1 1 d R U . O5W O 0.1599(4) 0.4912(5) 0.9527(5) 0.0286(11) Uani 1 1 d . . . H5WA H 0.130392 0.403316 0.957937 0.034 Uiso 1 1 d R U . H5WB H 0.095082 0.514296 0.887687 0.034 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 Ni1 0.0151(6) 0.0121(6) 0.0125(5) 0.0020(4) 0.0018(4) 0.0034(4) Ni2 0.0193(4) 0.0119(4) 0.0114(4) 0.0039(3) 0.0009(3) 0.0002(3) P1 0.0111(7) 0.0114(8) 0.0104(7) 0.0039(6) 0.0005(6) 0.0021(6) P2 0.0154(8) 0.0118(8) 0.0102(7) 0.0035(6) -0.0006(6) 0.0025(6) C1 0.012(3) 0.008(3) 0.013(3) 0.003(2) 0.001(2) 0.005(2) C2 0.014(3) 0.017(3) 0.013(3) 0.007(3) 0.001(2) 0.002(2) C3 0.019(3) 0.015(3) 0.036(4) 0.010(3) 0.002(3) 0.003(3) C4 0.014(3) 0.032(4) 0.038(4) 0.011(3) 0.006(3) 0.003(3) C5 0.023(3) 0.017(3) 0.028(3) 0.011(3) 0.004(3) -0.002(3) C6 0.014(3) 0.017(3) 0.022(3) 0.005(3) 0.003(2) 0.000(2) N1 0.018(3) 0.033(3) 0.014(2) 0.009(2) -0.003(2) -0.008(2) O1 0.0111(19) 0.008(2) 0.0158(19) 0.0019(17) 0.0066(15) 0.0039(16) O2 0.018(2) 0.011(2) 0.0106(18) 0.0017(17) -0.0019(15) -0.0011(17) O3 0.016(2) 0.010(2) 0.0118(19) 0.0015(17) 0.0005(15) 0.0022(17) O4 0.012(2) 0.018(2) 0.020(2) 0.0099(18) 0.0022(16) 0.0045(17) O5 0.013(2) 0.014(2) 0.0146(19) 0.0027(17) -0.0009(16) 0.0028(17) O6 0.027(2) 0.013(2) 0.0066(18) 0.0002(17) 0.0000(16) -0.0022(18) O7 0.020(2) 0.023(2) 0.021(2) 0.0065(19) -0.0002(17) 0.0069(19) O1W 0.030(2) 0.018(2) 0.020(2) 0.0017(19) 0.0094(18) 0.003(2) O2W 0.030(3) 0.050(3) 0.025(2) 0.024(2) 0.003(2) -0.002(2) O3W 0.043(3) 0.021(3) 0.022(2) 0.009(2) -0.005(2) 0.008(2) O4W 0.119(5) 0.040(4) 0.040(3) 0.009(3) -0.023(3) 0.030(4) O5W 0.019(2) 0.033(3) 0.042(3) 0.026(2) 0.0006(19) 0.000(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' 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' Ni Ni 0.3393 1.1124 '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 Ni1 O3 180.0 2_766 . O3 Ni1 O5 90.90(14) 2_766 . O3 Ni1 O5 89.10(14) . . O3 Ni1 O5 89.10(14) 2_766 2_766 O3 Ni1 O5 90.90(14) . 2_766 O5 Ni1 O5 180.0 . 2_766 O3 Ni1 O1W 90.93(15) 2_766 2_766 O3 Ni1 O1W 89.07(15) . 2_766 O5 Ni1 O1W 87.03(15) . 2_766 O5 Ni1 O1W 92.96(15) 2_766 2_766 O3 Ni1 O1W 89.07(15) 2_766 . O3 Ni1 O1W 90.94(15) . . O5 Ni1 O1W 92.97(15) . . O5 Ni1 O1W 87.04(15) 2_766 . O1W Ni1 O1W 180.0 2_766 . O2 Ni2 O6 176.35(15) 2_777 . O2 Ni2 O2W 90.74(16) 2_777 . O6 Ni2 O2W 90.97(16) . . O2 Ni2 O4 92.84(15) 2_777 . O6 Ni2 O4 90.26(15) . . O2W Ni2 O4 93.84(16) . . O2 Ni2 O1 94.41(14) 2_777 . O6 Ni2 O1 84.16(15) . . O2W Ni2 O1 172.90(17) . . O4 Ni2 O1 81.05(14) . . O2 Ni2 O3W 84.79(16) 2_777 . O6 Ni2 O3W 91.85(16) . . O2W Ni2 O3W 95.09(18) . . O4 Ni2 O3W 170.79(16) . . O1 Ni2 O3W 90.25(16) . . O3 P1 O2 109.8(2) . . O3 P1 O4 113.3(2) . . O2 P1 O4 112.2(2) . . O3 P1 C1 112.3(2) . . O2 P1 C1 106.1(2) . . O4 P1 C1 102.7(2) . . O7 P2 O5 113.1(2) . . O7 P2 O6 112.7(2) . . O5 P2 O6 111.4(2) . . O7 P2 C1 109.5(2) . . O5 P2 C1 107.7(2) . . O6 P2 C1 101.9(2) . . O1 C1 C2 109.6(4) . . O1 C1 P2 104.1(3) . . C2 C1 P2 117.0(4) . . O1 C1 P1 103.4(3) . . C2 C1 P1 111.6(4) . . P2 C1 P1 110.0(3) . . C3 C2 C6 108.8(4) . . C3 C2 C1 114.5(5) . . C6 C2 C1 114.2(4) . . C3 C2 H2 106.2 . . C6 C2 H2 106.2 . . C1 C2 H2 106.2 . . C4 C3 C2 110.4(5) . . 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 110.6(5) . . N1 C4 H4A 109.5 . . C3 C4 H4A 109.5 . . N1 C4 H4B 109.5 . . C3 C4 H4B 109.5 . . H4A C4 H4B 108.1 . . N1 C5 C6 112.0(5) . . N1 C5 H5A 109.2 . . C6 C5 H5A 109.2 . . N1 C5 H5B 109.2 . . C6 C5 H5B 109.2 . . H5A C5 H5B 107.9 . . C5 C6 C2 109.2(5) . . C5 C6 H6A 109.8 . . C2 C6 H6A 109.8 . . C5 C6 H6B 109.8 . . C2 C6 H6B 109.8 . . H6A C6 H6B 108.3 . . C4 N1 C5 112.4(4) . . C4 N1 H1A 109.1 . . C5 N1 H1A 109.1 . . C4 N1 H1B 109.1 . . C5 N1 H1B 109.1 . . H1A N1 H1B 107.9 . . C1 O1 Ni2 104.5(3) . . C1 O1 H1C 127.7 . . Ni2 O1 H1C 127.8 . . P1 O2 Ni2 130.1(2) . 2_777 P1 O3 Ni1 129.2(2) . . P1 O4 Ni2 115.6(2) . . P2 O5 Ni1 129.3(2) . . P2 O6 Ni2 116.3(2) . . Ni1 O1W H1WB 109.3 . . Ni1 O1W H1WA 108.9 . . H1WB O1W H1WA 109.4 . . Ni2 O2W H2WA 109.5 . . Ni2 O2W H2WB 109.1 . . H2WA O2W H2WB 109.6 . . Ni2 O3W H3WB 109.9 . . Ni2 O3W H3WA 109.7 . . H3WB O3W H3WA 108.9 . . H4WA O4W H4WB 112.7 . . H5WA O5W H5WB 112.4 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 O3 2.043(3) 2_766 Ni1 O3 2.043(3) . Ni1 O5 2.067(4) . Ni1 O5 2.067(4) 2_766 Ni1 O1W 2.090(4) 2_766 Ni1 O1W 2.090(4) . Ni2 O2 2.001(4) 2_777 Ni2 O6 2.020(4) . Ni2 O2W 2.046(4) . Ni2 O4 2.086(4) . Ni2 O1 2.104(4) . Ni2 O3W 2.115(4) . P1 O3 1.510(4) . P1 O2 1.516(4) . P1 O4 1.531(4) . P1 C1 1.862(5) . P2 O7 1.494(4) . P2 O5 1.523(4) . P2 O6 1.537(4) . P2 C1 1.842(5) . C1 O1 1.457(6) . C1 C2 1.535(7) . C2 C3 1.523(7) . C2 C6 1.526(8) . C2 H2 0.9800 . C3 C4 1.507(8) . C3 H3A 0.9700 . C3 H3B 0.9700 . C4 N1 1.482(8) . C4 H4A 0.9700 . C4 H4B 0.9700 . C5 N1 1.484(7) . C5 C6 1.501(8) . 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 0.8433 . O1W H1WA 0.8419 . O2W H2WA 0.8470 . O2W H2WB 0.8430 . O3W H3WB 0.8445 . O3W H3WA 0.8434 . O4W H4WA 0.8905 . O4W H4WB 0.8964 . O5W H5WA 0.8899 . O5W H5WB 0.8956 . 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 2.888(5) 162.9 1_455 yes O5W H5WB O2 0.90 2.57 3.093(6) 118.0 1_455 yes O5W H5WA O2 0.89 2.00 2.879(6) 168.8 2_667 yes O4W H4WB O7 0.90 1.87 2.695(6) 152.4 2_666 yes O4W H4WA O7 0.89 1.96 2.837(7) 166.6 1_545 yes O3W H3WA O5W 0.84 2.21 2.975(6) 150.1 2_677 yes O3W H3WB O4W 0.84 2.19 2.839(8) 134.1 1_565 yes O2W H2WB O6 0.84 1.87 2.675(5) 160.5 2_776 yes O1W H1WA O6 0.84 2.39 2.881(5) 117.8 . yes O1W H1WA O4 0.84 2.28 3.045(5) 150.7 . yes O1W H1WB O3W 0.84 2.25 3.025(6) 153.0 2_776 yes N1 H1A O5 0.89 1.91 2.743(6) 154.9 2_666 yes N1 H1B O5W 0.89 1.96 2.835(6) 167.0 . yes C6 H6B O3 0.97 2.63 3.360(6) 132.6 . yes C5 H5B O5W 0.97 2.64 3.346(7) 129.5 2_667 yes C5 H5A O4W 0.97 2.41 3.345(8) 162.4 . yes C5 H5A O7 0.97 2.52 3.236(7) 131.0 2_666 yes C4 H4B O4 0.97 2.34 3.306(7) 172.4 1_455 yes C3 H3B O7 0.97 2.43 3.073(7) 123.9 . yes C2 H2 O2 0.98 2.52 3.011(6) 110.5 . yes O5W H5WB O3 0.90 2.02 2.888(5) 162.9 1_455 yes O5W H5WB O2 0.90 2.57 3.093(6) 118.0 1_455 yes O5W H5WA O2 0.89 2.00 2.879(6) 168.8 2_667 yes O4W H4WB O7 0.90 1.87 2.695(6) 152.4 2_666 yes O4W H4WA O7 0.89 1.96 2.837(7) 166.6 1_545 yes O3W H3WA O5W 0.84 2.21 2.975(6) 150.1 2_677 yes O3W H3WB O4W 0.84 2.19 2.839(8) 134.1 1_565 yes O2W H2WB O6 0.84 1.87 2.675(5) 160.5 2_776 yes O1W H1WA O6 0.84 2.39 2.881(5) 117.8 . yes O1W H1WA O4 0.84 2.28 3.045(5) 150.7 . yes O1W H1WB O3W 0.84 2.25 3.025(6) 153.0 2_776 yes N1 H1A O5 0.89 1.91 2.743(6) 154.9 2_666 yes N1 H1B O5W 0.89 1.96 2.835(6) 167.0 . yes C6 H6B O3 0.97 2.63 3.360(6) 132.6 . yes C5 H5B O5W 0.97 2.64 3.346(7) 129.5 2_667 yes C5 H5A O4W 0.97 2.41 3.345(8) 162.4 . yes C5 H5A O7 0.97 2.52 3.236(7) 131.0 2_666 yes C4 H4B O4 0.97 2.34 3.306(7) 172.4 1_455 yes C3 H3B O7 0.97 2.43 3.073(7) 123.9 . yes C2 H2 O2 0.98 2.52 3.011(6) 110.5 . yes O5W H5WB O3 0.90 2.02 2.888(5) 162.9 1_455 yes O5W H5WB O2 0.90 2.57 3.093(6) 118.0 1_455 yes O5W H5WA O2 0.89 2.00 2.879(6) 168.8 2_667 yes O4W H4WB O7 0.90 1.87 2.695(6) 152.4 2_666 yes O4W H4WA O7 0.89 1.96 2.837(7) 166.6 1_545 yes O3W H3WB O4W 0.84 2.19 2.839(8) 134.1 1_565 yes O3W H3WA O5W 0.84 2.21 2.975(6) 150.1 2_677 yes O2W H2WB O6 0.84 1.87 2.675(5) 160.5 2_776 yes O1W H1WA O6 0.84 2.39 2.881(5) 117.8 . yes O1W H1WA O4 0.84 2.28 3.045(5) 150.7 . yes O1W H1WB O3W 0.84 2.25 3.025(6) 153.0 2_776 yes N1 H1A O5 0.89 1.91 2.743(6) 154.9 2_666 yes N1 H1B O5W 0.89 1.96 2.835(6) 167.0 . yes C6 H6B O3 0.97 2.63 3.360(6) 132.6 . yes C5 H5B O5W 0.97 2.64 3.346(7) 129.5 2_667 yes C5 H5A O4W 0.97 2.41 3.345(8) 162.4 . yes C5 H5A O7 0.97 2.52 3.236(7) 131.0 2_666 yes C4 H4B O4 0.97 2.34 3.306(7) 172.4 1_455 yes C3 H3B O7 0.97 2.43 3.073(7) 123.9 . yes C2 H2 O2 0.98 2.52 3.011(6) 110.5 . yes C2 H2 O2 0.98 2.52 3.011(6) 110.5 . yes C3 H3B O7 0.97 2.43 3.073(7) 123.9 . yes C4 H4B O4 0.97 2.34 3.306(7) 172.4 1_455 yes C5 H5A O7 0.97 2.52 3.236(7) 131.0 2_666 yes C5 H5A O4W 0.97 2.41 3.345(8) 162.4 . yes C5 H5B O5W 0.97 2.64 3.346(7) 129.5 2_667 yes C6 H6B O3 0.97 2.63 3.360(6) 132.6 . yes N1 H1B O5W 0.89 1.96 2.835(6) 167.0 . yes N1 H1A O5 0.89 1.91 2.743(6) 154.9 2_666 yes O1W H1WB O3W 0.84 2.25 3.025(6) 153.0 2_776 yes O1W H1WA O4 0.84 2.28 3.045(5) 150.7 . yes O1W H1WA O6 0.84 2.39 2.881(5) 117.8 . yes O2W H2WB O6 0.84 1.87 2.675(5) 160.5 2_776 yes O3W H3WA O5W 0.84 2.21 2.975(6) 150.1 2_677 yes O3W H3WB O4W 0.84 2.19 2.839(8) 134.1 1_565 yes O4W H4WA O7 0.89 1.96 2.837(7) 166.6 1_545 yes O4W H4WB O7 0.90 1.87 2.695(6) 152.4 2_666 yes O5W H5WA O2 0.89 2.00 2.879(6) 168.8 2_667 yes O5W H5WB O2 0.90 2.57 3.093(6) 118.0 1_455 yes O5W H5WB O3 0.90 2.02 2.888(5) 162.9 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 -73.1(4) . O5 P2 C1 O1 163.6(3) . O6 P2 C1 O1 46.4(3) . O7 P2 C1 C2 48.0(5) . O5 P2 C1 C2 -75.4(4) . O6 P2 C1 C2 167.4(4) . O7 P2 C1 P1 176.7(3) . O5 P2 C1 P1 53.4(3) . O6 P2 C1 P1 -63.9(3) . O3 P1 C1 O1 -161.8(3) . O2 P1 C1 O1 78.2(4) . O4 P1 C1 O1 -39.8(3) . O3 P1 C1 C2 80.5(4) . O2 P1 C1 C2 -39.5(4) . O4 P1 C1 C2 -157.5(4) . O3 P1 C1 P2 -51.1(3) . O2 P1 C1 P2 -171.1(2) . O4 P1 C1 P2 71.0(3) . O1 C1 C2 C3 53.4(6) . P2 C1 C2 C3 -64.8(6) . P1 C1 C2 C3 167.3(4) . O1 C1 C2 C6 179.8(4) . P2 C1 C2 C6 61.6(6) . P1 C1 C2 C6 -66.3(5) . C6 C2 C3 C4 59.5(6) . C1 C2 C3 C4 -171.4(5) . C2 C3 C4 N1 -57.1(6) . N1 C5 C6 C2 57.1(6) . C3 C2 C6 C5 -58.8(6) . C1 C2 C6 C5 171.9(4) . C3 C4 N1 C5 54.7(7) . C6 C5 N1 C4 -55.5(6) . C2 C1 O1 Ni2 178.1(3) . P2 C1 O1 Ni2 -56.0(3) . P1 C1 O1 Ni2 59.0(3) . O3 P1 O2 Ni2 141.0(3) 2_777 O4 P1 O2 Ni2 14.0(4) 2_777 C1 P1 O2 Ni2 -97.4(3) 2_777 O2 P1 O3 Ni1 170.2(2) . O4 P1 O3 Ni1 -63.4(3) . C1 P1 O3 Ni1 52.4(3) . O3 P1 O4 Ni2 122.8(2) . O2 P1 O4 Ni2 -112.1(2) . C1 P1 O4 Ni2 1.5(3) . O7 P2 O5 Ni1 177.6(3) . O6 P2 O5 Ni1 49.6(3) . C1 P2 O5 Ni1 -61.3(3) . O7 P2 O6 Ni2 103.5(3) . O5 P2 O6 Ni2 -128.2(2) . C1 P2 O6 Ni2 -13.7(3) .