# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_coden_Cambridge 440 _publ_contact_author_name 'Yong Fan' _publ_contact_author_email MRFY@JLU.EDU.CN _publ_section_title ; Solvothermal syntheses, characterizations and properties of three transition-metal (NiII, CoII) carboxylate-phosphonates ; loop_ _publ_author_name 'Yong Fan.' 'Kui-Rong Ma.' 'Jing Shi.' 'Tian-Yong Song.' 'Jianing Xu.' ; L.-r.Zhang ; 'Daojun Zhang.' 'Yulan Zhu.' data_H3O[CoH2L2(H2O)2]2H2O_(3) _database_code_depnum_ccdc_archive 'CCDC 610098' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C4 H19 Co N O13 P2' _chemical_formula_sum 'C4 H19 Co N O13 P2' _chemical_formula_weight 410.07 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3817(19) _cell_length_b 9.3988(19) _cell_length_c 9.776(2) _cell_angle_alpha 82.84(3) _cell_angle_beta 62.55(3) _cell_angle_gamma 76.32(3) _cell_volume 743.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3405 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 1.435 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.676 _exptl_absorpt_correction_T_max 0.729 _exptl_absorpt_process_details Process-auto _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7382 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3405 _reflns_number_gt 3097 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.8581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3405 _refine_ls_number_parameters 233 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.003 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.46158(3) 0.15623(3) 0.22156(3) 0.01738(10) Uani 1 1 d . . . P2 P 0.13439(7) 0.10823(6) 0.24197(6) 0.01912(13) Uani 1 1 d . . . P1 P 0.48149(8) 0.47173(6) 0.26281(7) 0.02211(14) Uani 1 1 d . . . O1 O 0.5492(2) 0.1884(2) -0.01628(19) 0.0305(4) Uani 1 1 d D . . O2 O 0.3782(2) 0.12674(18) 0.45529(18) 0.0244(3) Uani 1 1 d . . . O3 O 0.5840(2) 0.31733(18) 0.2246(2) 0.0267(4) Uani 1 1 d . . . O4 O 0.1019(2) 0.0723(2) 0.1139(2) 0.0277(4) Uani 1 1 d . . . O5 O 0.6553(2) -0.0229(2) 0.1791(2) 0.0358(5) Uani 1 1 d . . . N1 N 0.2435(2) 0.3318(2) 0.2939(2) 0.0186(4) Uani 1 1 d . . . O6 O 0.30017(19) 0.02537(17) 0.23146(19) 0.0232(3) Uani 1 1 d . . . O7 O -0.0086(2) 0.0906(2) 0.4019(2) 0.0322(4) Uani 1 1 d D . . O8 O 0.4140(3) 0.5044(3) 0.4343(2) 0.0459(6) Uani 1 1 d D . . C2 C 0.3013(3) 0.4712(2) 0.2367(3) 0.0228(4) Uani 1 1 d . . . H3 H 0.2142 0.5522 0.2919 0.027 Uiso 1 1 calc R . . H4 H 0.3282 0.4847 0.1281 0.027 Uiso 1 1 calc R . . O9 O 0.5663(3) 0.5879(2) 0.1584(3) 0.0492(6) Uani 1 1 d . . . O10W O 0.1016(3) 0.7881(3) 0.0175(3) 0.0516(6) Uani 1 1 d D . . C1 C 0.1449(3) 0.3015(2) 0.2220(3) 0.0210(4) Uani 1 1 d . . . H2 H 0.1938 0.3289 0.1135 0.025 Uiso 1 1 calc R . . H1 H 0.0348 0.3603 0.2706 0.025 Uiso 1 1 calc R . . C4 C 0.1561(3) 0.3241(3) 0.4650(2) 0.0236(5) Uani 1 1 d . . . H5 H 0.0470 0.3077 0.4957 0.028 Uiso 1 1 calc R . . H6 H 0.1437 0.4179 0.5052 0.028 Uiso 1 1 calc R . . O11 O 0.1702(3) 0.1931(3) 0.6811(2) 0.0546(7) Uani 1 1 d . . . C3 C 0.2415(3) 0.2047(3) 0.5384(3) 0.0248(5) Uani 1 1 d . . . O12W O 0.6447(4) 0.1807(3) 0.5131(4) 0.0636(8) Uani 1 1 d D . . O13W O 0.8769(4) 0.5602(4) 0.1417(4) 0.0663(7) Uani 1 1 d . . . H14 H 0.043(5) 0.832(5) -0.035(5) 0.080 Uiso 1 1 d D . . H13 H 0.203(3) 0.734(4) -0.046(4) 0.058(11) Uiso 1 1 d D . . H10 H 0.692(4) -0.063(4) 0.231(4) 0.036(9) Uiso 1 1 d . . . H11 H 0.719(5) -0.044(4) 0.090(5) 0.054(11) Uiso 1 1 d . . . H7 H 0.503(4) 0.268(2) -0.050(4) 0.049(10) Uiso 1 1 d D . . H8 H 0.605(4) 0.112(3) -0.073(4) 0.059 Uiso 1 1 d D . . H16 H 0.766(5) 0.152(4) 0.462(4) 0.059 Uiso 1 1 d . . . H18 H 0.764(4) 0.591(4) 0.159(4) 0.059 Uiso 1 1 d D . . H17 H 0.603(5) 0.107(3) 0.508(5) 0.059 Uiso 1 1 d D . . H19 H 0.949(4) 0.526(5) 0.061(4) 0.059 Uiso 1 1 d D . . H15 H 0.050(5) 0.730(4) 0.096(3) 0.059 Uiso 1 1 d D . . H9 H 0.033(4) 0.024(4) 0.447(4) 0.059 Uiso 1 1 d D . . H12 H 0.501(3) 0.500(5) 0.448(4) 0.059 Uiso 1 1 d D . . 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 0.01729(16) 0.01735(16) 0.01613(16) -0.00087(10) -0.00794(12) 0.00017(11) P2 0.0172(3) 0.0226(3) 0.0175(3) -0.0004(2) -0.0085(2) -0.0023(2) P1 0.0296(3) 0.0175(3) 0.0241(3) -0.0004(2) -0.0170(3) -0.0028(2) O1 0.0421(10) 0.0242(9) 0.0195(8) -0.0022(7) -0.0139(8) 0.0044(8) O2 0.0253(8) 0.0255(8) 0.0203(8) 0.0026(6) -0.0122(7) 0.0013(6) O3 0.0202(8) 0.0230(8) 0.0354(9) -0.0069(7) -0.0110(7) -0.0013(6) O4 0.0274(8) 0.0345(9) 0.0265(8) -0.0036(7) -0.0159(7) -0.0062(7) O5 0.0328(10) 0.0400(11) 0.0229(9) -0.0042(8) -0.0131(9) 0.0168(8) N1 0.0210(9) 0.0189(9) 0.0166(8) -0.0001(7) -0.0107(7) -0.0003(7) O6 0.0214(8) 0.0207(8) 0.0291(8) -0.0039(6) -0.0137(7) -0.0004(6) O7 0.0245(9) 0.0381(10) 0.0240(9) 0.0076(7) -0.0060(7) -0.0031(7) O8 0.0448(12) 0.0621(14) 0.0366(11) -0.0243(10) -0.0278(10) 0.0117(10) C2 0.0292(11) 0.0182(10) 0.0247(11) 0.0019(8) -0.0171(10) -0.0017(8) O9 0.0604(14) 0.0359(11) 0.0783(16) 0.0303(11) -0.0528(13) -0.0277(10) O10W 0.0361(12) 0.0661(16) 0.0443(13) 0.0040(11) -0.0152(11) -0.0038(11) C1 0.0223(10) 0.0223(11) 0.0203(10) 0.0011(8) -0.0133(9) -0.0008(8) C4 0.0226(11) 0.0277(12) 0.0165(10) -0.0038(8) -0.0080(9) 0.0020(9) O11 0.0405(12) 0.0823(17) 0.0173(9) 0.0092(10) -0.0074(9) 0.0125(11) C3 0.0258(11) 0.0301(12) 0.0174(10) 0.0017(9) -0.0102(9) -0.0036(9) O12W 0.0560(15) 0.0411(14) 0.109(2) 0.0022(14) -0.0496(16) -0.0116(11) O13W 0.0545(16) 0.077(2) 0.0705(19) -0.0100(15) -0.0319(15) -0.0054(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.0509(17) . ? Co1 O5 2.084(2) . ? Co1 O1 2.0865(18) . ? Co1 O3 2.1161(17) . ? Co1 O6 2.1286(17) . ? Co1 N1 2.184(2) . ? P2 O4 1.5099(17) . ? P2 O6 1.5284(17) . ? P2 O7 1.5422(19) . ? P2 C1 1.823(2) . ? P1 O9 1.500(2) . ? P1 O3 1.5214(18) . ? P1 O8 1.537(2) . ? P1 C2 1.823(2) . ? O1 H7 0.877(17) . ? O1 H8 0.864(17) . ? O2 C3 1.259(3) . ? O5 H10 0.76(4) . ? O5 H11 0.81(4) . ? N1 C2 1.483(3) . ? N1 C1 1.485(3) . ? N1 C4 1.487(3) . ? O7 H9 0.847(19) . ? O8 H12 0.876(19) . ? C2 H3 0.9700 . ? C2 H4 0.9700 . ? O10W H14 0.917(19) . ? O10W H13 0.923(19) . ? O10W H15 0.894(19) . ? C1 H2 0.9700 . ? C1 H1 0.9700 . ? C4 C3 1.524(3) . ? C4 H5 0.9700 . ? C4 H6 0.9700 . ? O11 C3 1.241(3) . ? O12W H16 0.99(4) . ? O12W H17 0.892(19) . ? O13W H18 0.97(4) . ? O13W H19 0.81(3) . ? 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 _geom_angle_publ_flag O2 Co1 O5 91.51(8) . . ? O2 Co1 O1 179.01(8) . . ? O5 Co1 O1 88.41(9) . . ? O2 Co1 O3 89.69(8) . . ? O5 Co1 O3 97.30(8) . . ? O1 Co1 O3 89.34(8) . . ? O2 Co1 O6 88.82(7) . . ? O5 Co1 O6 93.01(8) . . ? O1 Co1 O6 92.17(8) . . ? O3 Co1 O6 169.62(6) . . ? O2 Co1 N1 82.01(7) . . ? O5 Co1 N1 172.98(8) . . ? O1 Co1 N1 98.11(8) . . ? O3 Co1 N1 85.41(7) . . ? O6 Co1 N1 84.21(7) . . ? O4 P2 O6 113.17(10) . . ? O4 P2 O7 111.65(11) . . ? O6 P2 O7 112.36(10) . . ? O4 P2 C1 107.80(10) . . ? O6 P2 C1 105.42(10) . . ? O7 P2 C1 105.87(12) . . ? O9 P1 O3 113.72(13) . . ? O9 P1 O8 112.54(15) . . ? O3 P1 O8 111.54(12) . . ? O9 P1 C2 108.29(11) . . ? O3 P1 C2 105.04(10) . . ? O8 P1 C2 104.97(12) . . ? Co1 O1 H7 118(2) . . ? Co1 O1 H8 117(2) . . ? H7 O1 H8 123(3) . . ? C3 O2 Co1 116.26(15) . . ? P1 O3 Co1 116.06(9) . . ? Co1 O5 H10 131(3) . . ? Co1 O5 H11 119(3) . . ? H10 O5 H11 109(4) . . ? C2 N1 C1 112.36(17) . . ? C2 N1 C4 112.11(18) . . ? C1 N1 C4 112.00(18) . . ? C2 N1 Co1 106.86(13) . . ? C1 N1 Co1 106.03(13) . . ? C4 N1 Co1 106.99(13) . . ? P2 O6 Co1 116.14(9) . . ? P2 O7 H9 105(2) . . ? P1 O8 H12 105(2) . . ? N1 C2 P1 111.13(14) . . ? N1 C2 H3 109.4 . . ? P1 C2 H3 109.4 . . ? N1 C2 H4 109.4 . . ? P1 C2 H4 109.4 . . ? H3 C2 H4 108.0 . . ? H14 O10W H13 113(4) . . ? H14 O10W H15 114(4) . . ? H13 O10W H15 108(4) . . ? N1 C1 P2 111.11(14) . . ? N1 C1 H2 109.4 . . ? P2 C1 H2 109.4 . . ? N1 C1 H1 109.4 . . ? P2 C1 H1 109.4 . . ? H2 C1 H1 108.0 . . ? N1 C4 C3 114.37(18) . . ? N1 C4 H5 108.7 . . ? C3 C4 H5 108.7 . . ? N1 C4 H6 108.7 . . ? C3 C4 H6 108.7 . . ? H5 C4 H6 107.6 . . ? O11 C3 O2 123.9(2) . . ? O11 C3 C4 116.1(2) . . ? O2 C3 C4 120.03(19) . . ? H16 O12W H17 109(3) . . ? H18 O13W H19 122(4) . . ? 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 O13W H19 O13W 0.81(3) 2.01(3) 2.818(7) 178(4) 2_765 O12W H16 O7 0.99(4) 1.88(4) 2.855(3) 169(3) 1_655 O1 H8 O6 0.864(17) 1.89(2) 2.725(3) 164(3) 2_655 O1 H7 O9 0.877(17) 1.80(2) 2.666(3) 167(3) 2_665 O5 H11 O4 0.81(4) 1.93(4) 2.725(3) 168(4) 2_655 O5 H10 O11 0.76(4) 1.98(4) 2.718(3) 166(4) 2_656 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.480 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.079 data_(H3O)3[NiL2(H2O)2]4H2O_(2) _database_code_depnum_ccdc_archive 'CCDC 610099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C4 H27 N Ni O17 P2' _chemical_formula_sum 'C4 H27 N Ni O17 P2' _chemical_formula_weight 481.92 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.568(2) _cell_length_b 10.689(2) _cell_length_c 15.816(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.17(3) _cell_angle_gamma 90.00 _cell_volume 1847.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4226 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.305 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.741 _exptl_absorpt_process_details Process-auto _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17748 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4226 _reflns_number_gt 3642 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+2.7871P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4226 _refine_ls_number_parameters 304 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.68313(3) 0.12201(3) 0.10137(2) 0.01441(10) Uani 1 1 d . . . P1 P 0.76004(6) -0.06741(6) -0.01832(4) 0.01625(14) Uani 1 1 d . . . P2 P 0.77230(6) 0.39566(6) 0.11162(5) 0.01941(15) Uani 1 1 d . . . O1 O 0.69195(16) -0.05657(16) 0.05057(12) 0.0190(4) Uani 1 1 d . . . O2 O 0.88086(17) -0.13594(18) 0.01988(14) 0.0268(4) Uani 1 1 d . . . O3 O 0.67827(17) -0.12261(17) -0.10653(13) 0.0242(4) Uani 1 1 d . . . O4 O 0.67582(16) 0.31431(17) 0.13325(12) 0.0209(4) Uani 1 1 d . . . O5 O 0.72456(19) 0.52323(18) 0.07296(14) 0.0295(4) Uani 1 1 d . . . O6 O 0.88942(18) 0.4042(2) 0.19092(14) 0.0296(5) Uani 1 1 d . . . O7 O 0.83315(16) 0.09168(19) 0.21118(12) 0.0248(4) Uani 1 1 d . . . O8 O 1.0355(2) 0.1075(3) 0.26192(15) 0.0470(7) Uani 1 1 d . . . O9 O 0.57035(17) 0.07275(19) 0.17279(13) 0.0245(4) Uani 1 1 d D . . H9A H 0.584(4) 0.010(3) 0.211(2) 0.051(11) Uiso 1 1 d D . . H9B H 0.4923(18) 0.078(3) 0.147(2) 0.035(9) Uiso 1 1 d D . . O10 O 0.53628(17) 0.15434(19) -0.01072(14) 0.0262(4) Uani 1 1 d D . . H10A H 0.517(3) 0.231(2) -0.032(2) 0.040(10) Uiso 1 1 d D . . H10B H 0.463(2) 0.120(4) -0.026(3) 0.057(13) Uiso 1 1 d D . . O1W O 0.8872(4) -0.4520(5) -0.1777(4) 0.1142(17) Uani 1 1 d D . . H1A H 0.963(3) -0.443(5) -0.185(3) 0.083(16) Uiso 1 1 d D . . H1B H 0.871(5) -0.535(2) -0.192(4) 0.080 Uiso 1 1 d D . . O2W O 1.0312(3) -0.1836(4) 0.1905(2) 0.0687(9) Uani 1 1 d D . . H2A H 0.990(4) -0.152(4) 0.1353(19) 0.080 Uiso 1 1 d D . . H2B H 1.041(5) -0.260(2) 0.168(3) 0.080 Uiso 1 1 d D . . O3W O 1.2480(3) 0.1894(4) 0.2461(2) 0.0674(10) Uani 1 1 d D . . H3A H 1.175(3) 0.162(5) 0.250(3) 0.083(16) Uiso 1 1 d D . . H3B H 1.222(5) 0.265(3) 0.223(4) 0.080 Uiso 1 1 d D . . H3C H 1.258(4) 0.161(4) 0.1946(19) 0.061(13) Uiso 1 1 d D . . O4W O 0.8833(3) -0.3823(2) -0.0124(3) 0.0712(11) Uani 1 1 d D . . H4A H 0.880(4) -0.301(2) -0.003(3) 0.075(15) Uiso 1 1 d D . . H4B H 0.832(4) -0.412(4) 0.014(3) 0.076(15) Uiso 1 1 d D . . O5W O 0.4311(2) 0.3660(3) 0.1120(2) 0.0471(6) Uani 1 1 d D . . H5A H 0.513(2) 0.349(3) 0.111(2) 0.040(10) Uiso 1 1 d D . . H5B H 0.430(4) 0.408(4) 0.166(2) 0.070(14) Uiso 1 1 d D . . H5C H 0.386(4) 0.290(3) 0.106(3) 0.068(14) Uiso 1 1 d D . . O6W O 0.7834(3) -0.2416(3) 0.18319(17) 0.0484(6) Uani 1 1 d D . . H6A H 0.746(3) -0.176(3) 0.142(2) 0.046(11) Uiso 1 1 d D . . H6B H 0.761(4) -0.326(2) 0.163(3) 0.080 Uiso 1 1 d D . . H6C H 0.789(4) -0.222(5) 0.2428(17) 0.080 Uiso 1 1 d D . . O7W O 0.5110(2) 0.6186(2) 0.07947(15) 0.0357(5) Uani 1 1 d D . . H7A H 0.509(3) 0.617(3) 0.1353(15) 0.037(10) Uiso 1 1 d D . . H7B H 0.582(3) 0.580(4) 0.081(3) 0.057(13) Uiso 1 1 d D . . N1 N 0.81501(18) 0.17257(19) 0.04129(13) 0.0154(4) Uani 1 1 d . . . C1 C 0.7894(2) 0.0951(2) -0.04093(17) 0.0185(5) Uani 1 1 d . . . H1C H 0.8588 0.0987 -0.0624 0.080 Uiso 1 1 calc . . . H1D H 0.7187 0.1286 -0.0874 0.080 Uiso 1 1 calc . . . C2 C 0.8017(2) 0.3089(2) 0.02117(17) 0.0191(5) Uani 1 1 d . . . H2C H 0.7347 0.3222 -0.0341 0.080 Uiso 1 1 calc . . . H2D H 0.8760 0.3401 0.0129 0.080 Uiso 1 1 calc . . . C3 C 0.9372(2) 0.1432(3) 0.10691(17) 0.0215(5) Uani 1 1 d . . . H3D H 0.9910 0.2140 0.1108 0.080 Uiso 1 1 calc . . . H3E H 0.9714 0.0722 0.0851 0.080 Uiso 1 1 calc . . . C4 C 0.9342(3) 0.1132(3) 0.20018(19) 0.0269(6) Uani 1 1 d . . . 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 0.01437(16) 0.01509(17) 0.01468(16) 0.00016(12) 0.00603(12) -0.00141(11) P1 0.0176(3) 0.0135(3) 0.0187(3) -0.0009(2) 0.0073(2) -0.0007(2) P2 0.0225(3) 0.0153(3) 0.0228(3) -0.0039(2) 0.0107(3) -0.0035(2) O1 0.0212(9) 0.0161(9) 0.0222(9) 0.0005(7) 0.0105(7) -0.0023(7) O2 0.0218(9) 0.0231(10) 0.0355(11) 0.0027(8) 0.0095(8) 0.0057(8) O3 0.0257(10) 0.0224(10) 0.0246(10) -0.0072(8) 0.0082(8) -0.0043(7) O4 0.0233(9) 0.0180(9) 0.0249(9) -0.0029(7) 0.0127(7) -0.0031(7) O5 0.0370(11) 0.0162(9) 0.0404(12) -0.0014(8) 0.0195(9) -0.0013(8) O6 0.0257(10) 0.0349(11) 0.0276(10) -0.0130(9) 0.0079(8) -0.0061(8) O7 0.0182(9) 0.0369(11) 0.0189(9) 0.0039(8) 0.0057(7) -0.0003(8) O8 0.0204(11) 0.091(2) 0.0266(11) 0.0106(12) 0.0029(9) -0.0020(11) O9 0.0183(9) 0.0316(11) 0.0257(10) 0.0104(8) 0.0100(8) 0.0007(8) O10 0.0201(10) 0.0238(10) 0.0287(10) 0.0065(8) -0.0004(8) -0.0034(8) O1W 0.082(3) 0.146(4) 0.134(4) -0.058(3) 0.062(3) -0.065(3) O2W 0.0477(16) 0.110(3) 0.0497(17) 0.0288(18) 0.0177(14) 0.0203(18) O3W 0.0445(16) 0.123(3) 0.0412(16) -0.0331(18) 0.0233(13) -0.0398(18) O4W 0.102(3) 0.0250(14) 0.125(3) -0.0001(16) 0.090(2) 0.0021(15) O5W 0.0445(14) 0.0425(15) 0.0591(17) -0.0087(13) 0.0237(13) -0.0038(12) O6W 0.0620(17) 0.0456(15) 0.0351(13) 0.0068(12) 0.0126(12) -0.0019(13) O7W 0.0422(13) 0.0352(12) 0.0288(11) 0.0084(10) 0.0103(10) 0.0082(10) N1 0.0181(10) 0.0141(10) 0.0152(10) -0.0007(8) 0.0070(8) -0.0023(8) C1 0.0252(13) 0.0156(12) 0.0167(11) -0.0002(9) 0.0094(10) -0.0020(9) C2 0.0267(13) 0.0154(12) 0.0180(12) -0.0013(9) 0.0114(10) -0.0041(10) C3 0.0182(12) 0.0278(14) 0.0195(12) 0.0007(10) 0.0075(10) -0.0007(10) C4 0.0214(13) 0.0373(16) 0.0213(13) 0.0029(12) 0.0061(11) 0.0007(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O7 2.038(2) . ? Ni1 O10 2.042(2) . ? Ni1 O9 2.0550(19) . ? Ni1 O1 2.0866(18) . ? Ni1 N1 2.115(2) . ? Ni1 O4 2.1246(19) . ? P1 O2 1.517(2) . ? P1 O3 1.524(2) . ? P1 O1 1.5442(19) . ? P1 C1 1.828(3) . ? P2 O6 1.517(2) . ? P2 O5 1.522(2) . ? P2 O4 1.5393(19) . ? P2 C2 1.828(3) . ? O7 C4 1.258(3) . ? O8 C4 1.256(4) . ? O9 H9A 0.880(19) . ? O9 H9B 0.861(18) . ? O10 H10A 0.884(18) . ? O10 H10B 0.880(19) . ? O1W H1A 0.92(2) . ? O1W H1B 0.91(2) . ? O2W H2A 0.911(19) . ? O2W H2B 0.912(19) . ? O3W H3A 0.910(19) . ? O3W H3B 0.892(19) . ? O3W H3C 0.912(19) . ? O4W H4A 0.880(19) . ? O4W H4B 0.89(2) . ? O5W H5A 0.975(18) . ? O5W H5B 0.969(19) . ? O5W H5C 0.954(19) . ? O6W H6A 0.958(19) . ? O6W H6B 0.96(2) . ? O6W H6C 0.949(19) . ? O7W H7A 0.891(18) . ? O7W H7B 0.910(19) . ? N1 C3 1.487(3) . ? N1 C1 1.487(3) . ? N1 C2 1.488(3) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.521(4) . ? C3 H3D 0.9700 . ? C3 H3E 0.9700 . ? 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 _geom_angle_publ_flag O7 Ni1 O10 178.23(8) . . ? O7 Ni1 O9 90.43(8) . . ? O10 Ni1 O9 91.33(8) . . ? O7 Ni1 O1 92.69(8) . . ? O10 Ni1 O1 87.28(8) . . ? O9 Ni1 O1 95.59(8) . . ? O7 Ni1 N1 83.42(8) . . ? O10 Ni1 N1 94.81(8) . . ? O9 Ni1 N1 173.76(8) . . ? O1 Ni1 N1 85.82(7) . . ? O7 Ni1 O4 92.34(8) . . ? O10 Ni1 O4 87.46(8) . . ? O9 Ni1 O4 92.04(8) . . ? O1 Ni1 O4 170.83(7) . . ? N1 Ni1 O4 87.15(7) . . ? O2 P1 O3 113.04(12) . . ? O2 P1 O1 111.84(11) . . ? O3 P1 O1 111.59(10) . . ? O2 P1 C1 109.33(12) . . ? O3 P1 C1 106.75(11) . . ? O1 P1 C1 103.72(11) . . ? O6 P2 O5 112.71(12) . . ? O6 P2 O4 111.47(12) . . ? O5 P2 O4 113.67(11) . . ? O6 P2 C2 109.40(12) . . ? O5 P2 C2 106.06(12) . . ? O4 P2 C2 102.84(11) . . ? P1 O1 Ni1 116.17(10) . . ? P2 O4 Ni1 113.92(10) . . ? C4 O7 Ni1 115.03(18) . . ? Ni1 O9 H9A 125(3) . . ? Ni1 O9 H9B 119(2) . . ? H9A O9 H9B 107(3) . . ? Ni1 O10 H10A 121(2) . . ? Ni1 O10 H10B 128(3) . . ? H10A O10 H10B 101(3) . . ? H1A O1W H1B 101(5) . . ? H2A O2W H2B 93(2) . . ? H3A O3W H3B 97(5) . . ? H3A O3W H3C 109(4) . . ? H3B O3W H3C 93(4) . . ? H4A O4W H4B 101(4) . . ? H5A O5W H5B 114(4) . . ? H5A O5W H5C 110(4) . . ? H5B O5W H5C 109(4) . . ? H6A O6W H6B 117(4) . . ? H6A O6W H6C 112(4) . . ? H6B O6W H6C 117(4) . . ? H7A O7W H7B 106(4) . . ? C3 N1 C1 111.3(2) . . ? C3 N1 C2 111.34(19) . . ? C1 N1 C2 112.39(19) . . ? C3 N1 Ni1 107.03(15) . . ? C1 N1 Ni1 106.53(14) . . ? C2 N1 Ni1 107.89(15) . . ? N1 C1 P1 110.76(16) . . ? N1 C1 H1C 109.5 . . ? P1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? P1 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? N1 C2 P2 111.22(16) . . ? N1 C2 H2C 109.4 . . ? P2 C2 H2C 109.4 . . ? N1 C2 H2D 109.4 . . ? P2 C2 H2D 109.4 . . ? H2C C2 H2D 108.0 . . ? N1 C3 C4 113.8(2) . . ? N1 C3 H3D 108.8 . . ? C4 C3 H3D 108.8 . . ? N1 C3 H3E 108.8 . . ? C4 C3 H3E 108.8 . . ? H3D C3 H3E 107.7 . . ? O8 C4 O7 123.7(3) . . ? O8 C4 C3 116.9(2) . . ? O7 C4 C3 119.4(2) . . ? 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 O9 H9A O6 0.880(19) 1.86(2) 2.730(3) 168(4) 2_645 O9 H9B O3 0.861(18) 1.92(2) 2.770(3) 168(4) 3_655 O10 H10A O7W 0.884(18) 1.761(19) 2.642(3) 174(4) 3_665 O10 H10B O1 0.880(19) 1.84(2) 2.714(3) 175(4) 3_655 O1W H1A O6 0.92(2) 1.80(2) 2.709(4) 171(5) 3_755 O1W H1B O3W 0.91(2) 2.20(3) 3.035(6) 152(5) 4 O2W H2A O2 0.911(19) 1.85(2) 2.735(4) 162(4) . O3W H3A O8 0.910(19) 1.79(2) 2.697(4) 177(5) . O3W H3B O1W 0.892(19) 2.35(3) 3.222(8) 165(5) 3_755 O3W H3C O3 0.912(19) 1.82(2) 2.710(4) 163(4) 3_755 O4W H4A O2 0.880(19) 1.81(2) 2.685(3) 177(5) . O4W H4B O5 0.89(2) 1.92(2) 2.801(4) 179(5) 1_545 O5W H5A O4 0.975(18) 1.83(2) 2.795(3) 169(3) . O5W H5B O8 0.969(19) 2.39(3) 3.206(4) 142(4) 2_655 O5W H5B O2W 0.969(19) 2.38(4) 3.055(4) 126(3) 2_655 O5W H5C O3 0.954(19) 1.94(2) 2.882(3) 170(4) 3_655 O6W H6A O1 0.958(19) 1.88(2) 2.824(3) 170(4) . O6W H6B O5 0.96(2) 2.10(3) 3.007(3) 156(4) 1_545 O6W H6C O4 0.949(19) 1.91(2) 2.848(3) 172(4) 2_645 O7W H7A O8 0.891(18) 1.86(2) 2.736(3) 166(3) 2_655 O7W H7A O7 0.891(18) 2.53(3) 3.221(3) 135(3) 2_655 O7W H7B O5 0.910(19) 1.80(2) 2.705(3) 171(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.614 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.083 # Attachment 'CIF_compounds_1-3.CIF' data_[NH3(CH2)3NH3](NH4)4[NiL2(H2O))]2_(1) _database_code_depnum_ccdc_archive 'CCDC 629612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C11 H44 N8 Ni2 O18 P4' _chemical_formula_sum 'C11 H44 N8 Ni2 O18 P4' _chemical_formula_weight 817.84 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -c2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.315(2) _cell_length_b 19.282(4) _cell_length_c 14.432(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.01(3) _cell_angle_gamma 90.00 _cell_volume 3067.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3526 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.715 _exptl_absorpt_process_details Process-auto _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15025 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3526 _reflns_number_gt 3065 _reflns_threshold_expression >2sigma(I) _computing_data_collection Process-auto _computing_cell_refinement Process-auto _computing_data_reduction Process-auto _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+5.6086P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3526 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.62014(2) 0.460473(13) 0.021735(18) 0.01151(8) Uani 1 1 d . . . P1 P 0.65476(5) 0.61664(3) 0.06631(4) 0.01275(12) Uani 1 1 d . . . P2 P 0.83226(5) 0.35875(3) 0.08342(4) 0.01468(12) Uani 1 1 d . . . N1 N 0.79687(15) 0.49973(9) 0.06544(12) 0.0122(3) Uani 1 1 d . . . N2 N 0.54904(14) 0.27318(7) 0.09092(10) 0.0240(4) Uani 1 1 d . . . H4 H 0.4834 0.2986 0.0679 0.036 Uiso 1 1 calc R . . H5 H 0.5616 0.2441 0.0462 0.036 Uiso 1 1 calc R . . H6 H 0.6131 0.3009 0.1086 0.036 Uiso 1 1 calc R . . N3 N 0.61561(16) 0.67622(7) 0.33874(9) 0.0241(4) Uani 1 1 d R . . N4 N 0.16050(12) 0.30614(9) 0.13008(10) 0.0214(4) Uani 1 1 d R . . C1 C 0.78982(19) 0.56532(11) 0.11758(16) 0.0168(4) Uani 1 1 d . . . H1A H 0.8615 0.5929 0.1174 0.025 Uiso 1 1 calc R . . H1B H 0.7897 0.5546 0.1832 0.025 Uiso 1 1 calc R . . C2 C 0.87373(18) 0.44680(11) 0.12751(14) 0.0146(4) Uani 1 1 d . . . H2A H 0.8629 0.4511 0.1921 0.022 Uiso 1 1 calc R . . H2B H 0.9585 0.4552 0.1285 0.022 Uiso 1 1 calc R . . C3 C 0.83885(19) 0.51110(12) -0.02340(15) 0.0174(4) Uani 1 1 d . . . H3A H 0.8918 0.4731 -0.0314 0.026 Uiso 1 1 calc R . . H3B H 0.8866 0.5533 -0.0167 0.026 Uiso 1 1 calc R . . C4 C 0.7375(2) 0.51675(11) -0.11330(15) 0.0173(4) Uani 1 1 d . . . C5 C 0.5310(3) 0.23347(14) 0.1734(2) 0.0429(8) Uani 1 1 d . . . H5A H 0.6044 0.2077 0.1999 0.064 Uiso 1 1 calc R . . H5B H 0.4662 0.2002 0.1523 0.064 Uiso 1 1 calc R . . C6 C 0.5000 0.27809(19) 0.2500 0.0278(8) Uani 1 2 d S . . H6A H 0.4315 0.3076 0.2228 0.042 Uiso 0.50 1 calc PR . . H6B H 0.5685 0.3076 0.2772 0.042 Uiso 0.50 1 calc PR . . O1 O 0.55684(13) 0.56068(7) 0.03850(11) 0.0157(3) Uani 1 1 d . . . O2 O 0.63293(15) 0.66221(8) 0.14687(11) 0.0207(3) Uani 1 1 d . . . O3 O 0.67263(15) 0.65820(8) -0.01812(12) 0.0236(4) Uani 1 1 d . . . O4 O 0.70554(14) 0.36745(8) 0.01827(11) 0.0203(3) Uani 1 1 d . . . O5 O 0.82695(19) 0.31384(9) 0.16877(12) 0.0318(4) Uani 1 1 d . . . O6 O 0.92396(15) 0.33402(9) 0.02848(12) 0.0266(4) Uani 1 1 d . . . O7 O 0.63655(14) 0.48917(8) -0.11162(11) 0.0193(3) Uani 1 1 d . . . O8 O 0.76302(16) 0.54518(10) -0.18395(12) 0.0299(4) Uani 1 1 d . . . O9 O 0.58579(17) 0.43558(9) 0.15499(12) 0.0218(4) Uani 1 1 d . . . H1 H 0.528(3) 0.4537(15) 0.156(2) 0.031(9) Uiso 1 1 d . . . H2 H 0.640(3) 0.4442(18) 0.213(3) 0.056(10) Uiso 1 1 d . . . H7 H 0.541(3) 0.6716(14) 0.3405(19) 0.027(7) Uiso 1 1 d . . . H8 H 0.633(3) 0.6539(17) 0.281(2) 0.050(9) Uiso 1 1 d . . . H9 H 0.657(3) 0.6607(17) 0.394(2) 0.047(10) Uiso 1 1 d . . . H10 H 0.632(3) 0.7270(18) 0.338(2) 0.048(9) Uiso 1 1 d . . . H11 H 0.214(3) 0.3220(16) 0.100(2) 0.038(8) Uiso 1 1 d . . . H12 H 0.161(3) 0.2615(16) 0.133(2) 0.034(8) Uiso 1 1 d . . . H13 H 0.081(4) 0.3208(18) 0.099(3) 0.061(11) Uiso 1 1 d . . . H14 H 0.169(3) 0.3235(18) 0.189(3) 0.057(11) Uiso 1 1 d . . . 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 0.00906(13) 0.01146(13) 0.01430(14) -0.00042(10) 0.00321(10) 0.00034(9) P1 0.0116(2) 0.0110(2) 0.0165(3) -0.0009(2) 0.0048(2) 0.00004(19) P2 0.0157(3) 0.0139(3) 0.0146(3) 0.0001(2) 0.0037(2) 0.0041(2) N1 0.0116(8) 0.0137(8) 0.0117(8) -0.0003(7) 0.0032(6) 0.0015(6) N2 0.0266(11) 0.0252(10) 0.0237(10) 0.0014(9) 0.0126(8) 0.0005(8) N3 0.0257(12) 0.0281(11) 0.0186(10) 0.0005(9) 0.0051(9) -0.0044(9) N4 0.0218(11) 0.0172(10) 0.0260(11) 0.0017(9) 0.0072(9) -0.0012(8) C1 0.0127(10) 0.0140(10) 0.0216(11) -0.0037(9) -0.0007(8) 0.0005(8) C2 0.0106(9) 0.0188(10) 0.0133(10) 0.0001(8) 0.0003(8) 0.0042(8) C3 0.0127(10) 0.0225(11) 0.0182(11) 0.0033(9) 0.0060(8) 0.0006(8) C4 0.0182(11) 0.0200(10) 0.0155(10) 0.0006(9) 0.0073(8) 0.0010(9) C5 0.079(2) 0.0264(13) 0.0316(15) 0.0043(12) 0.0310(15) 0.0034(14) C6 0.035(2) 0.0275(18) 0.0225(17) 0.000 0.0113(15) 0.000 O1 0.0109(7) 0.0120(7) 0.0239(8) -0.0009(6) 0.0035(6) 0.0013(5) O2 0.0254(9) 0.0180(7) 0.0201(8) -0.0048(7) 0.0079(7) 0.0027(6) O3 0.0244(9) 0.0242(8) 0.0252(9) 0.0077(7) 0.0118(7) 0.0008(7) O4 0.0165(8) 0.0151(7) 0.0273(9) -0.0052(7) 0.0002(6) 0.0029(6) O5 0.0587(13) 0.0179(8) 0.0198(8) 0.0033(7) 0.0108(8) 0.0016(8) O6 0.0202(8) 0.0313(9) 0.0299(9) -0.0099(8) 0.0087(7) 0.0064(7) O7 0.0149(7) 0.0265(8) 0.0169(7) 0.0006(7) 0.0048(6) -0.0017(6) O8 0.0262(9) 0.0472(11) 0.0171(8) 0.0072(8) 0.0065(7) -0.0087(8) O9 0.0187(9) 0.0285(9) 0.0196(9) 0.0029(7) 0.0071(7) 0.0045(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.0367(15) 5_665 ? Ni1 O4 2.0433(15) . ? Ni1 O7 2.0507(16) . ? Ni1 O1 2.0936(15) . ? Ni1 N1 2.0980(18) . ? Ni1 O9 2.1016(17) . ? P1 O3 1.5096(17) . ? P1 O2 1.5212(16) . ? P1 O1 1.5338(15) . ? P1 C1 1.831(2) . ? P2 O6 1.5176(17) . ? P2 O5 1.5179(17) . ? P2 O4 1.5365(17) . ? P2 C2 1.837(2) . ? N1 C3 1.480(3) . ? N1 C1 1.483(3) . ? N1 C2 1.500(3) . ? N2 C5 1.467(3) . ? N2 H4 0.8900 . ? N2 H5 0.8900 . ? N2 H6 0.8900 . ? N3 H7 0.85(3) . ? N3 H8 0.99(3) . ? N3 H9 0.88(3) . ? N3 H10 1.00(3) . ? N4 H11 0.87(3) . ? N4 H12 0.86(3) . ? N4 H13 0.95(4) . ? N4 H14 0.90(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.530(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O8 1.247(3) . ? C4 O7 1.265(3) . ? C5 C6 1.504(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.504(3) 2_655 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O1 Ni1 2.0367(15) 5_665 ? O9 H1 0.74(3) . ? O9 H2 0.93(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 _geom_angle_publ_flag O1 Ni1 O4 103.81(6) 5_665 . ? O1 Ni1 O7 86.65(7) 5_665 . ? O4 Ni1 O7 94.05(7) . . ? O1 Ni1 O1 84.55(6) 5_665 . ? O4 Ni1 O1 171.48(6) . . ? O7 Ni1 O1 88.00(6) . . ? O1 Ni1 N1 168.39(6) 5_665 . ? O4 Ni1 N1 84.27(6) . . ? O7 Ni1 N1 84.44(7) . . ? O1 Ni1 N1 87.70(6) . . ? O1 Ni1 O9 88.75(7) 5_665 . ? O4 Ni1 O9 90.45(7) . . ? O7 Ni1 O9 174.22(7) . . ? O1 Ni1 O9 88.07(7) . . ? N1 Ni1 O9 99.64(7) . . ? O3 P1 O2 112.61(9) . . ? O3 P1 O1 112.48(9) . . ? O2 P1 O1 111.98(9) . . ? O3 P1 C1 111.21(10) . . ? O2 P1 C1 105.53(10) . . ? O1 P1 C1 102.33(9) . . ? O6 P2 O5 113.66(11) . . ? O6 P2 O4 111.61(10) . . ? O5 P2 O4 110.90(11) . . ? O6 P2 C2 108.67(10) . . ? O5 P2 C2 107.45(10) . . ? O4 P2 C2 103.97(9) . . ? C3 N1 C1 112.19(17) . . ? C3 N1 C2 111.22(16) . . ? C1 N1 C2 111.56(16) . . ? C3 N1 Ni1 105.25(12) . . ? C1 N1 Ni1 107.68(12) . . ? C2 N1 Ni1 108.61(12) . . ? C5 N2 H4 109.5 . . ? C5 N2 H5 109.5 . . ? H4 N2 H5 109.5 . . ? C5 N2 H6 109.5 . . ? H4 N2 H6 109.5 . . ? H5 N2 H6 109.5 . . ? H7 N3 H8 112(3) . . ? H7 N3 H9 106(3) . . ? H8 N3 H9 116(3) . . ? H7 N3 H10 107(3) . . ? H8 N3 H10 110(3) . . ? H9 N3 H10 106(3) . . ? H11 N4 H12 112(3) . . ? H11 N4 H13 110(3) . . ? H12 N4 H13 108(3) . . ? H11 N4 H14 113(3) . . ? H12 N4 H14 109(3) . . ? H13 N4 H14 103(3) . . ? N1 C1 P1 113.03(14) . . ? N1 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N1 C2 P2 110.71(13) . . ? N1 C2 H2A 109.5 . . ? P2 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? P2 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N1 C3 C4 114.82(17) . . ? N1 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N1 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? O8 C4 O7 125.2(2) . . ? O8 C4 C3 117.22(19) . . ? O7 C4 C3 117.47(19) . . ? N2 C5 C6 113.3(2) . . ? N2 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C5 110.2(3) . 2_655 ? C5 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 2_655 . ? C5 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 2_655 . ? H6A C6 H6B 108.1 . . ? P1 O1 Ni1 146.66(9) . 5_665 ? P1 O1 Ni1 115.71(8) . . ? Ni1 O1 Ni1 95.45(6) 5_665 . ? P2 O4 Ni1 117.53(9) . . ? C4 O7 Ni1 113.85(14) . . ? Ni1 O9 H1 105(2) . . ? Ni1 O9 H2 124(2) . . ? H1 O9 H2 107(3) . . ? 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 N2 H4 O3 0.89 1.94 2.821(2) 171.7 5_665 N2 H5 O6 0.89 1.88 2.752(2) 165.6 7_655 N2 H6 O4 0.89 2.25 2.894(2) 129.1 . N2 H6 O5 0.89 2.39 3.190(3) 149.1 . O9 H1 O7 0.74(3) 2.14(3) 2.849(2) 161(3) 5_665 O9 H2 O8 0.93(4) 1.81(4) 2.732(3) 171(3) 6_566 N3 H7 O2 0.85(3) 2.03(3) 2.879(2) 177(3) 2_655 N3 H8 O2 0.99(3) 1.95(3) 2.833(2) 147(3) . N3 H9 O4 0.88(3) 1.84(3) 2.696(2) 164(3) 6_566 N3 H10 O5 1.00(3) 1.74(3) 2.740(2) 175(3) 4_655 N4 H11 O3 0.87(3) 1.97(3) 2.832(2) 169(3) 5_665 N4 H12 O2 0.86(3) 1.96(3) 2.809(2) 169(3) 3_445 N4 H13 O6 0.95(4) 1.86(4) 2.799(2) 170(3) 1_455 N4 H14 O5 0.90(4) 2.05(4) 2.878(2) 152(3) 2_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.375 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.079