Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Petr Hermann' 'Vojtech Kubicek' 'Ivan Lukes' 'Jakub Rudovsky' 'Pavel Vojtisek' _publ_contact_author_name 'Dr Petr Hermann' _publ_contact_author_address ; Department of Inorganic Chemistry Universita Karlova Hlavova 2030 Prague 2 128 43 CZECH REPUBLIC ; _publ_contact_author_email PETRH@NATUR.CUNI.CZ _publ_section_title ; Complexes of divalent transition metal ions with bis(aminomethyl)phosphinic acid in aqueous solution and in the solid state ; data_ca5end _database_code_CSD 211306 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Ca(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Ca(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety (Ca((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_sum 'C4 H24 Ca Cl4 N4 O6 P2' _chemical_formula_weight 468.09 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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)/c _symmetry_Int_Tables_number 14 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 8.4190(2) _cell_length_b 7.9000(2) _cell_length_c 13.6270(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.4230(14) _cell_angle_gamma 90.00 _cell_volume 885.11(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.58 _cell_measurement_theta_max 27.50 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.7mm _exptl_crystal_size_mid 0.35mm _exptl_crystal_size_min 0.4mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3784 _diffrn_reflns_av_R_equivalents 0.0102 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1991 _reflns_number_gt 1887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0194P)^2^+0.3798P] 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 SHELXL _refine_ls_extinction_coef 0.017(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1991 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.000 _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 Ca Ca 0.0000 0.0000 0.0000 0.00988(11) Uani 1 2 d S . . Cl1 Cl -0.25983(4) 0.01871(4) 0.08395(2) 0.01688(10) Uani 1 1 d . . . O3W O 0.04606(12) 0.29403(11) 0.01229(7) 0.0186(2) Uani 1 1 d . . . H1W H 0.059(2) 0.356(3) 0.0649(15) 0.045(5) Uiso 1 1 d . . . H2W H 0.105(2) 0.341(3) -0.0262(15) 0.049(6) Uiso 1 1 d . . . P P -0.32880(4) 0.01470(3) -0.21829(2) 0.00863(10) Uani 1 1 d . . . O1 O -0.15846(9) 0.04495(11) -0.15788(6) 0.01196(18) Uani 1 1 d . . . O2 O -0.34943(10) -0.01199(10) -0.32921(6) 0.01275(19) Uani 1 1 d . . . C1 C -0.45360(14) 0.19470(15) -0.19702(8) 0.0126(2) Uani 1 1 d . . . H11 H -0.5588(18) 0.1556(18) -0.1949(10) 0.015(3) Uiso 1 1 d . . . H12 H -0.4571(18) 0.2738(19) -0.2513(11) 0.018(4) Uiso 1 1 d . . . C2 C -0.41090(14) -0.16856(14) -0.16450(8) 0.0113(2) Uani 1 1 d . . . H21 H -0.3232(18) -0.2521(19) -0.1465(10) 0.015(3) Uiso 1 1 d . . . H22 H -0.4513(18) -0.1339(19) -0.1087(11) 0.019(4) Uiso 1 1 d . . . N1 N -0.38584(13) 0.28422(13) -0.10076(8) 0.0142(2) Uani 1 1 d . . . H11N H -0.462(2) 0.353(2) -0.0880(12) 0.025(4) Uiso 1 1 d . . . H12N H -0.358(2) 0.212(2) -0.0457(13) 0.031(4) Uiso 1 1 d . . . H13N H -0.296(2) 0.345(2) -0.1086(12) 0.028(4) Uiso 1 1 d . . . N2 N -0.54860(12) -0.24993(13) -0.23657(8) 0.0134(2) Uani 1 1 d . . . H21N H -0.603(2) -0.319(2) -0.2019(12) 0.026(4) Uiso 1 1 d . . . H22N H -0.619(2) -0.175(2) -0.2722(12) 0.028(4) Uiso 1 1 d . . . H23N H -0.505(2) -0.310(2) -0.2833(13) 0.032(4) Uiso 1 1 d . . . Cl2 Cl 0.29025(4) 0.49109(3) -0.10827(2) 0.01470(10) 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 Ca 0.00960(18) 0.01104(17) 0.00887(17) 0.00055(10) 0.00175(13) 0.00033(10) Cl1 0.01543(17) 0.02001(18) 0.01744(18) 0.00368(10) 0.00850(13) 0.00393(10) O3W 0.0304(5) 0.0123(4) 0.0138(4) -0.0012(3) 0.0060(4) -0.0027(4) P 0.00864(17) 0.00850(16) 0.00888(17) 0.00027(9) 0.00220(12) 0.00022(9) O1 0.0108(4) 0.0133(4) 0.0114(4) 0.0007(3) 0.0016(3) -0.0007(3) O2 0.0144(4) 0.0142(4) 0.0096(4) -0.0002(3) 0.0023(3) 0.0003(3) C1 0.0132(6) 0.0109(5) 0.0134(5) 0.0001(4) 0.0025(4) 0.0009(4) C2 0.0123(5) 0.0106(5) 0.0111(5) 0.0004(4) 0.0026(4) -0.0007(4) N1 0.0170(5) 0.0122(5) 0.0143(5) -0.0013(4) 0.0052(4) 0.0029(4) N2 0.0127(5) 0.0122(5) 0.0149(5) 0.0010(4) 0.0022(4) -0.0019(4) Cl2 0.01464(17) 0.01322(16) 0.01675(17) -0.00091(9) 0.00452(12) -0.00110(10) _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 Ca O1 2.3020(8) 3 ? Ca O1 2.3020(8) . ? Ca O3W 2.3550(9) . ? Ca O3W 2.3550(9) 3 ? Ca Cl1 2.6818(3) . ? Ca Cl1 2.6818(3) 3 ? O3W H1W 0.86(2) . ? O3W H2W 0.88(2) . ? P O2 1.4988(9) . ? P O1 1.5111(8) . ? P C2 1.8246(12) . ? P C1 1.8279(12) . ? C1 N1 1.4914(15) . ? C1 H11 0.944(14) . ? C1 H12 0.963(15) . ? C2 N2 1.4939(14) . ? C2 H21 0.981(15) . ? C2 H22 0.938(15) . ? N1 H11N 0.886(17) . ? N1 H12N 0.930(18) . ? N1 H13N 0.925(18) . ? N2 H21N 0.907(17) . ? N2 H22N 0.902(18) . ? N2 H23N 0.929(18) . ? 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 Ca O1 180.00(5) 3 . ? O1 Ca O3W 91.85(3) 3 . ? O1 Ca O3W 88.15(3) . . ? O1 Ca O3W 88.15(3) 3 3 ? O1 Ca O3W 91.85(3) . 3 ? O3W Ca O3W 180.0 . 3 ? O1 Ca Cl1 88.38(2) 3 . ? O1 Ca Cl1 91.62(2) . . ? O3W Ca Cl1 93.00(2) . . ? O3W Ca Cl1 87.00(2) 3 . ? O1 Ca Cl1 91.62(2) 3 3 ? O1 Ca Cl1 88.38(2) . 3 ? O3W Ca Cl1 87.00(2) . 3 ? O3W Ca Cl1 93.00(2) 3 3 ? Cl1 Ca Cl1 180.000(17) . 3 ? Ca O3W H1W 127.8(13) . . ? Ca O3W H2W 118.9(14) . . ? H1W O3W H2W 105.6(18) . . ? O2 P O1 117.53(5) . . ? O2 P C2 108.77(5) . . ? O1 P C2 107.68(5) . . ? O2 P C1 108.88(5) . . ? O1 P C1 107.52(5) . . ? C2 P C1 105.85(6) . . ? P O1 Ca 140.90(5) . . ? N1 C1 P 112.59(8) . . ? N1 C1 H11 108.2(8) . . ? P C1 H11 108.9(9) . . ? N1 C1 H12 108.0(9) . . ? P C1 H12 107.9(9) . . ? H11 C1 H12 111.2(12) . . ? N2 C2 P 112.63(8) . . ? N2 C2 H21 108.1(8) . . ? P C2 H21 107.7(8) . . ? N2 C2 H22 107.0(9) . . ? P C2 H22 109.2(9) . . ? H21 C2 H22 112.2(12) . . ? C1 N1 H11N 107.9(10) . . ? C1 N1 H12N 113.6(10) . . ? H11N N1 H12N 106.5(14) . . ? C1 N1 H13N 108.2(10) . . ? H11N N1 H13N 110.6(14) . . ? H12N N1 H13N 110.0(14) . . ? C2 N2 H21N 108.8(10) . . ? C2 N2 H22N 113.2(11) . . ? H21N N2 H22N 109.3(14) . . ? C2 N2 H23N 108.0(11) . . ? H21N N2 H23N 111.5(15) . . ? H22N N2 H23N 106.0(14) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.372 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.048 data_cd9end _database_code_CSD 211307 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Cd(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Cd(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point (Cd((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_moiety ? _chemical_formula_sum 'C4 H24 Cd Cl4 N4 O6 P2' #(H-atoms on water molecule O3 were not found) _chemical_formula_weight 540.41 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' Cl Cl 0.1484 0.1585 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 8.3050(2) _cell_length_b 7.9080(2) _cell_length_c 13.5910(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.3860(13) _cell_angle_gamma 90.00 _cell_volume 871.83(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.54 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3mm _exptl_crystal_size_mid 0.3mm _exptl_crystal_size_min 0.052mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 2.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13964 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.54 _reflns_number_total 1997 _reflns_number_gt 1886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0309P)^2^+11.2365P] 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 SHELXL _refine_ls_extinction_coef 0.018(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1997 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.292 _refine_ls_restrained_S_all 1.292 _refine_ls_shift/su_max 0.000 _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 Cd Cd 0.0000 0.0000 0.0000 0.0095(3) Uani 1 2 d S . . Cl1 Cl -0.24891(17) 0.01672(19) 0.07986(11) 0.0156(3) Uani 1 1 d . . . P P 0.32893(17) -0.01833(18) 0.21679(11) 0.0090(3) Uani 1 1 d . . . O1 O 0.1538(5) -0.0461(5) 0.1581(3) 0.0119(8) Uani 1 1 d . . . O3W O 0.0340(6) 0.2932(5) 0.0099(3) 0.0167(9) Uani 1 1 d . . . O2 O 0.3518(5) 0.0058(5) 0.3273(3) 0.0125(8) Uani 1 1 d . . . N1 N 0.5474(6) 0.2490(7) 0.2370(4) 0.0137(10) Uani 1 1 d . . . H11N H 0.606(12) 0.322(13) 0.196(7) 0.04(3) Uiso 1 1 d . . . H12N H 0.619(13) 0.169(14) 0.267(8) 0.05(3) Uiso 1 1 d . . . H13N H 0.499(9) 0.317(10) 0.279(6) 0.016(18) Uiso 1 1 d . . . C1 C 0.4117(7) 0.1654(7) 0.1635(4) 0.0118(11) Uani 1 1 d . . . H11 H 0.457(10) 0.138(11) 0.106(6) 0.02(2) Uiso 1 1 d . . . H12 H 0.321(10) 0.258(11) 0.143(6) 0.02(2) Uiso 1 1 d . . . N2 N 0.3775(7) -0.2901(7) 0.0986(4) 0.0139(10) Uani 1 1 d . . . H21N H 0.461(12) -0.363(13) 0.087(7) 0.04(2) Uiso 1 1 d . . . H22N H 0.350(11) -0.211(13) 0.049(7) 0.04(2) Uiso 1 1 d . . . H23N H 0.291(11) -0.352(12) 0.108(7) 0.03(2) Uiso 1 1 d . . . C2 C 0.4531(7) -0.1982(7) 0.1934(4) 0.0132(11) Uani 1 1 d . . . H21 H 0.563(8) -0.156(9) 0.192(5) 0.008(16) Uiso 1 1 d . . . H22 H 0.467(10) -0.276(11) 0.251(6) 0.03(2) Uiso 1 1 d . . . Cl2 Cl 0.70994(18) 0.50898(17) 0.10835(11) 0.0149(3) 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 Cd 0.0093(3) 0.0114(4) 0.0079(3) 0.00078(19) 0.0017(2) 0.00081(19) Cl1 0.0133(6) 0.0191(7) 0.0162(7) 0.0041(5) 0.0070(5) 0.0040(5) P 0.0085(7) 0.0100(7) 0.0087(7) 0.0001(5) 0.0020(5) 0.0000(5) O1 0.0079(18) 0.017(2) 0.0120(19) -0.0041(16) 0.0043(15) -0.0032(15) O3W 0.027(2) 0.009(2) 0.013(2) 0.0005(15) 0.0044(17) -0.0005(17) O2 0.016(2) 0.010(2) 0.012(2) 0.0002(14) 0.0041(16) 0.0007(14) N1 0.012(2) 0.012(2) 0.017(2) 0.000(2) 0.0030(19) -0.0023(19) C1 0.012(2) 0.011(3) 0.013(3) -0.001(2) 0.003(2) -0.002(2) N2 0.016(2) 0.012(2) 0.015(2) -0.0020(19) 0.0059(19) 0.0018(19) C2 0.013(3) 0.012(3) 0.015(3) -0.001(2) 0.004(2) 0.001(2) Cl2 0.0147(7) 0.0140(7) 0.0169(7) -0.0010(5) 0.0050(5) -0.0011(5) _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 Cd O1 2.282(4) . ? Cd O1 2.282(4) 3 ? Cd O3W 2.336(4) . ? Cd O3W 2.336(4) 3 ? Cd Cl1 2.5360(14) 3 ? Cd Cl1 2.5360(14) . ? P O2 1.486(4) . ? P O1 1.517(4) . ? P C1 1.823(6) . ? P C2 1.824(6) . ? N1 C1 1.490(7) . ? N1 H11N 1.00(10) . ? N1 H12N 0.90(11) . ? N1 H13N 0.94(8) . ? C1 H11 0.96(8) . ? C1 H12 1.05(8) . ? N2 C2 1.495(8) . ? N2 H21N 0.94(10) . ? N2 H22N 0.91(10) . ? N2 H23N 0.90(10) . ? C2 H21 0.97(7) . ? C2 H22 0.98(9) . ? 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 Cd O1 180.0(3) . 3 ? O1 Cd O3W 93.91(15) . . ? O1 Cd O3W 86.09(15) 3 . ? O1 Cd O3W 86.09(15) . 3 ? O1 Cd O3W 93.91(15) 3 3 ? O3W Cd O3W 180.0(2) . 3 ? O1 Cd Cl1 92.97(10) . 3 ? O1 Cd Cl1 87.03(10) 3 3 ? O3W Cd Cl1 88.67(11) . 3 ? O3W Cd Cl1 91.33(11) 3 3 ? O1 Cd Cl1 87.03(10) . . ? O1 Cd Cl1 92.97(10) 3 . ? O3W Cd Cl1 91.33(11) . . ? O3W Cd Cl1 88.67(11) 3 . ? Cl1 Cd Cl1 180.00(5) 3 . ? O2 P O1 116.7(2) . . ? O2 P C1 108.8(3) . . ? O1 P C1 107.9(3) . . ? O2 P C2 108.8(3) . . ? O1 P C2 108.0(3) . . ? C1 P C2 106.1(3) . . ? P O1 Cd 138.7(2) . . ? C1 N1 H11N 106(5) . . ? C1 N1 H12N 109(7) . . ? H11N N1 H12N 108(8) . . ? C1 N1 H13N 108(5) . . ? H11N N1 H13N 110(7) . . ? H12N N1 H13N 116(8) . . ? N1 C1 P 112.5(4) . . ? N1 C1 H11 106(5) . . ? P C1 H11 113(5) . . ? N1 C1 H12 105(4) . . ? P C1 H12 111(4) . . ? H11 C1 H12 109(6) . . ? C2 N2 H21N 105(6) . . ? C2 N2 H22N 107(6) . . ? H21N N2 H22N 112(8) . . ? C2 N2 H23N 110(6) . . ? H21N N2 H23N 109(8) . . ? H22N N2 H23N 113(8) . . ? N2 C2 P 112.4(4) . . ? N2 C2 H21 112(4) . . ? P C2 H21 107(4) . . ? N2 C2 H22 110(5) . . ? P C2 H22 109(5) . . ? H21 C2 H22 107(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.482 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.191 data_c5end _database_code_CSD 211308 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Co(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Co(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety (Co((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_sum 'C4 H24 Cl4 Co N4 O6 P2' _chemical_formula_weight 486.94 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' Cl Cl 0.1484 0.1585 '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_Int_Tables_number 14 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 8.2740(2) _cell_length_b 7.9080(2) _cell_length_c 13.2520(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.0280(15) _cell_angle_gamma 90.00 _cell_volume 844.77(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data' _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 27.54 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.5mm _exptl_crystal_size_mid 0.5mm _exptl_crystal_size_min 0.4mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3686 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.54 _reflns_number_total 1922 _reflns_number_gt 1841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0339P)^2^+0.4540P] 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 SHELXL _refine_ls_extinction_coef 0.032(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1922 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Co Co 0.0000 0.0000 0.0000 0.01855(14) Uani 1 2 d S . . Cl1C Cl -0.23688(6) 0.01733(6) 0.08247(3) 0.02737(15) Uani 1 1 d . . . O3W O 0.02693(19) 0.26705(18) 0.01139(10) 0.0294(3) Uani 1 1 d . . . H1W H 0.021(5) 0.327(6) 0.062(3) 0.108(14) Uiso 1 1 d . . . H2W H 0.080(5) 0.320(5) -0.013(3) 0.101(14) Uiso 1 1 d . . . P P 0.32480(5) -0.00700(5) 0.21251(3) 0.01708(14) Uani 1 1 d . . . O1 O 0.15184(13) -0.03814(16) 0.14821(9) 0.0218(3) Uani 1 1 d . . . O2 O 0.34275(17) 0.01785(16) 0.32649(10) 0.0269(3) Uani 1 1 d . . . C1 C 0.45500(19) -0.1853(2) 0.19418(13) 0.0231(3) Uani 1 1 d . . . H11 H 0.455(3) -0.260(3) 0.2463(16) 0.027(5) Uiso 1 1 d . . . H12 H 0.559(3) -0.146(3) 0.1886(16) 0.034(6) Uiso 1 1 d . . . C2 C 0.4102(2) 0.1764(2) 0.15937(12) 0.0214(3) Uani 1 1 d . . . H21 H 0.322(3) 0.260(3) 0.1347(17) 0.032(6) Uiso 1 1 d . . . H22 H 0.453(3) 0.142(3) 0.1074(17) 0.037(6) Uiso 1 1 d . . . N1 N 0.3849(2) -0.2832(2) 0.09910(11) 0.0261(3) Uani 1 1 d . . . H11N H 0.293(3) -0.347(3) 0.1088(16) 0.032(5) Uiso 1 1 d . . . H12N H 0.466(3) -0.349(3) 0.0891(17) 0.041(6) Uiso 1 1 d . . . H13N H 0.344(3) -0.220(4) 0.052(2) 0.057(8) Uiso 1 1 d . . . N2 N 0.54647(18) 0.25961(19) 0.23590(11) 0.0246(3) Uani 1 1 d . . . H21N H 0.609(3) 0.329(3) 0.2020(18) 0.043(6) Uiso 1 1 d . . . H22N H 0.624(3) 0.185(4) 0.274(2) 0.054(7) Uiso 1 1 d . . . H23N H 0.504(3) 0.323(4) 0.279(2) 0.059(8) Uiso 1 1 d . . . Cl2 Cl 0.71951(6) 0.51287(5) 0.10309(4) 0.02811(15) 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 Co 0.01851(19) 0.0202(2) 0.01673(19) 0.00217(10) 0.00350(13) 0.00150(10) Cl1C 0.0251(2) 0.0335(3) 0.0255(2) 0.00732(15) 0.01001(17) 0.00602(15) O3W 0.0411(7) 0.0224(7) 0.0246(6) -0.0013(5) 0.0075(5) -0.0027(6) P 0.0166(2) 0.0176(2) 0.0175(2) 0.00019(12) 0.00489(16) -0.00032(13) O1 0.0183(5) 0.0251(6) 0.0214(6) 0.0020(5) 0.0030(4) -0.0013(5) O2 0.0285(6) 0.0339(7) 0.0189(6) -0.0020(4) 0.0065(5) -0.0015(5) C1 0.0212(7) 0.0205(8) 0.0275(8) 0.0023(6) 0.0051(6) 0.0023(6) C2 0.0234(7) 0.0194(8) 0.0215(7) 0.0007(6) 0.0051(6) -0.0022(6) N1 0.0319(7) 0.0235(8) 0.0237(7) 0.0006(6) 0.0084(6) 0.0079(7) N2 0.0241(7) 0.0220(7) 0.0261(7) 0.0009(6) 0.0025(6) -0.0042(6) Cl2 0.0277(3) 0.0263(3) 0.0295(2) -0.00295(14) 0.00484(17) -0.00285(15) _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 Co O1 2.1011(11) 3 ? Co O1 2.1011(11) . ? Co O3W 2.1253(15) 3 ? Co O3W 2.1253(15) . ? Co Cl1C 2.4536(4) . ? Co Cl1C 2.4536(4) 3 ? O3W H1W 0.83(4) . ? O3W H2W 0.74(4) . ? P O2 1.4969(13) . ? P O1 1.5116(11) . ? P C2 1.8230(16) . ? P C1 1.8238(17) . ? C1 N1 1.481(2) . ? C1 H11 0.91(2) . ? C1 H12 0.93(2) . ? C2 N2 1.489(2) . ? C2 H21 0.99(2) . ? C2 H22 0.89(2) . ? N1 H11N 0.95(2) . ? N1 H12N 0.88(3) . ? N1 H13N 0.81(3) . ? N2 H21N 0.94(3) . ? N2 H22N 0.93(3) . ? N2 H23N 0.89(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 O1 Co O1 180.00(8) 3 . ? O1 Co O3W 92.59(5) 3 3 ? O1 Co O3W 87.41(5) . 3 ? O1 Co O3W 87.41(5) 3 . ? O1 Co O3W 92.59(5) . . ? O3W Co O3W 180.00(7) 3 . ? O1 Co Cl1C 92.24(3) 3 . ? O1 Co Cl1C 87.76(3) . . ? O3W Co Cl1C 90.32(4) 3 . ? O3W Co Cl1C 89.68(4) . . ? O1 Co Cl1C 87.76(3) 3 3 ? O1 Co Cl1C 92.24(3) . 3 ? O3W Co Cl1C 89.68(4) 3 3 ? O3W Co Cl1C 90.32(4) . 3 ? Cl1C Co Cl1C 180.000(17) . 3 ? Co O3W H1W 127(3) . . ? Co O3W H2W 127(3) . . ? H1W O3W H2W 100(4) . . ? O2 P O1 117.14(7) . . ? O2 P C2 109.05(7) . . ? O1 P C2 108.17(7) . . ? O2 P C1 107.98(8) . . ? O1 P C1 108.15(7) . . ? C2 P C1 105.78(8) . . ? P O1 Co 142.58(7) . . ? N1 C1 P 112.81(11) . . ? N1 C1 H11 104.0(13) . . ? P C1 H11 107.6(13) . . ? N1 C1 H12 107.3(13) . . ? P C1 H12 109.6(14) . . ? H11 C1 H12 115.6(18) . . ? N2 C2 P 112.85(11) . . ? N2 C2 H21 108.8(13) . . ? P C2 H21 109.8(13) . . ? N2 C2 H22 106.8(15) . . ? P C2 H22 108.3(15) . . ? H21 C2 H22 110.4(19) . . ? C1 N1 H11N 109.8(13) . . ? C1 N1 H12N 105.8(15) . . ? H11N N1 H12N 111(2) . . ? C1 N1 H13N 110(2) . . ? H11N N1 H13N 103(2) . . ? H12N N1 H13N 116(2) . . ? C2 N2 H21N 110.5(14) . . ? C2 N2 H22N 114.3(17) . . ? H21N N2 H22N 104(2) . . ? C2 N2 H23N 109.4(18) . . ? H21N N2 H23N 109(2) . . ? H22N N2 H23N 110(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.401 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.067 data_coo2 _database_code_CSD 211309 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Co(L)2)ClO4*H2O (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common '(Co(L)2)ClO4*H2O (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H18 Cl Co N4 O9 P2' _chemical_formula_weight 422.54 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' Cl Cl 0.1484 0.1585 '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_Int_Tables_number 14 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 10.2410(3) _cell_length_b 9.4680(2) _cell_length_c 15.1850(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.4660(17) _cell_angle_gamma 90.00 _cell_volume 1425.68(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 27.54 _exptl_crystal_description irregular _exptl_crystal_colour 'brown orange' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6338 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3278 _reflns_number_gt 2898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0455P)^2^+0.5651P] 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 SHELXL _refine_ls_extinction_coef 0.0022(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3278 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _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 Co1 Co 0.00098(2) 0.19801(3) 0.256054(16) 0.01944(10) Uani 1 1 d . . . P1 P -0.04499(5) 0.45936(5) 0.31850(4) 0.02507(14) Uani 1 1 d . . . O11 O -0.12811(13) 0.32710(14) 0.27950(10) 0.0251(3) Uani 1 1 d . . . O12 O -0.12092(15) 0.58082(16) 0.34215(12) 0.0375(4) Uani 1 1 d . . . C11 C 0.0848(2) 0.3847(2) 0.41100(15) 0.0311(4) Uani 1 1 d . . . H111 H 0.163(3) 0.442(3) 0.4238(18) 0.040(7) Uiso 1 1 d . . . H112 H 0.055(3) 0.376(3) 0.4665(18) 0.037(7) Uiso 1 1 d . . . N11 N 0.11845(19) 0.24469(19) 0.37736(13) 0.0274(4) Uani 1 1 d . . . H113 H 0.106(3) 0.180(3) 0.4157(19) 0.037(7) Uiso 1 1 d . . . H114 H 0.193(3) 0.245(3) 0.374(2) 0.052(9) Uiso 1 1 d . . . C12 C 0.0445(2) 0.4956(2) 0.23183(17) 0.0314(5) Uani 1 1 d . . . H121 H -0.021(3) 0.537(3) 0.1770(18) 0.038(7) Uiso 1 1 d . . . H122 H 0.118(3) 0.553(3) 0.2536(19) 0.046(8) Uiso 1 1 d . . . N12 N 0.08991(18) 0.35484(18) 0.20750(14) 0.0269(4) Uani 1 1 d . . . H123 H 0.170(3) 0.342(3) 0.230(2) 0.045(8) Uiso 1 1 d . . . H124 H 0.072(3) 0.354(3) 0.145(2) 0.055(9) Uiso 1 1 d . . . P2 P 0.04325(5) -0.05511(5) 0.18259(4) 0.02432(13) Uani 1 1 d . . . O21 O 0.13029(13) 0.06906(14) 0.23001(10) 0.0259(3) Uani 1 1 d . . . O22 O 0.11576(16) -0.17527(15) 0.15242(12) 0.0354(4) Uani 1 1 d . . . C21 C -0.0783(3) 0.0339(2) 0.09276(15) 0.0339(5) Uani 1 1 d . . . H211 H -0.037(3) 0.061(3) 0.048(2) 0.058(9) Uiso 1 1 d . . . H212 H -0.152(3) -0.027(3) 0.067(2) 0.050(8) Uiso 1 1 d . . . N21 N -0.12178(17) 0.15958(18) 0.13640(12) 0.0242(3) Uani 1 1 d . . . H213 H -0.196(3) 0.147(3) 0.1424(18) 0.034(7) Uiso 1 1 d . . . H214 H -0.126(3) 0.230(3) 0.1007(18) 0.031(6) Uiso 1 1 d . . . C22 C -0.0549(2) -0.1012(2) 0.26272(15) 0.0274(4) Uani 1 1 d . . . H221 H -0.134(3) -0.146(3) 0.2338(18) 0.038(7) Uiso 1 1 d . . . H222 H 0.002(3) -0.158(3) 0.3135(18) 0.037(7) Uiso 1 1 d . . . N22 N -0.08494(19) 0.03599(18) 0.30231(13) 0.0267(4) Uani 1 1 d . . . H223 H -0.060(3) 0.029(3) 0.3598(19) 0.038(7) Uiso 1 1 d . . . H224 H -0.173(3) 0.044(3) 0.287(2) 0.052(8) Uiso 1 1 d . . . Cl1 Cl 0.29854(6) 0.33795(6) 0.00751(4) 0.03721(15) Uani 1 1 d . . . O1A O 0.4350(2) 0.3552(3) 0.00343(16) 0.0838(8) Uani 1 1 d . . . O2A O 0.2737(13) 0.4534(14) 0.0617(10) 0.068(3) Uani 0.60(5) 1 d P . . O2B O 0.265(2) 0.426(3) 0.0723(9) 0.066(4) Uani 0.40(5) 1 d P . . O3A O 0.2081(13) 0.3368(15) -0.0782(9) 0.069(3) Uani 0.60(5) 1 d P . . O3B O 0.2142(18) 0.377(4) -0.0810(13) 0.086(6) Uani 0.40(5) 1 d P . . O4A O 0.2777(12) 0.2093(11) 0.0561(9) 0.089(3) Uani 0.60(5) 1 d P . . O4B O 0.289(3) 0.2062(14) 0.025(3) 0.135(9) Uani 0.40(5) 1 d P . . O1W O 0.4387(2) 0.1484(2) 0.50508(14) 0.0449(4) Uani 1 1 d . . . H1W1 H 0.397(4) 0.097(4) 0.493(3) 0.077(15) Uiso 1 1 d . . . H1W2 H 0.440(4) 0.198(4) 0.458(3) 0.069(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 Co1 0.01527(15) 0.02011(16) 0.02354(16) -0.00147(9) 0.00599(11) -0.00075(9) P1 0.0187(2) 0.0220(2) 0.0351(3) -0.0027(2) 0.0078(2) 0.00133(18) O11 0.0178(6) 0.0257(7) 0.0326(7) -0.0029(6) 0.0077(6) 0.0001(5) O12 0.0285(7) 0.0281(7) 0.0587(10) -0.0064(7) 0.0162(7) 0.0057(6) C11 0.0298(11) 0.0309(10) 0.0302(11) -0.0080(8) 0.0026(9) 0.0006(9) N11 0.0231(9) 0.0259(9) 0.0312(9) -0.0019(7) 0.0032(7) 0.0024(7) C12 0.0278(10) 0.0233(10) 0.0449(13) 0.0051(9) 0.0124(10) 0.0000(8) N12 0.0217(9) 0.0266(8) 0.0346(10) -0.0013(7) 0.0107(8) -0.0029(7) P2 0.0206(2) 0.0228(3) 0.0304(3) -0.00295(19) 0.0081(2) 0.00172(18) O21 0.0181(6) 0.0253(7) 0.0357(8) -0.0028(6) 0.0095(6) -0.0003(5) O22 0.0315(8) 0.0288(7) 0.0491(10) -0.0077(7) 0.0159(7) 0.0056(6) C21 0.0411(12) 0.0325(11) 0.0264(11) -0.0062(9) 0.0050(9) 0.0061(9) N21 0.0202(8) 0.0259(8) 0.0268(9) 0.0000(7) 0.0063(7) 0.0014(7) C22 0.0252(10) 0.0228(9) 0.0352(11) -0.0008(8) 0.0094(8) -0.0029(8) N22 0.0246(9) 0.0279(9) 0.0303(9) -0.0021(7) 0.0120(7) -0.0020(7) Cl1 0.0383(3) 0.0395(3) 0.0323(3) -0.0051(2) 0.0061(2) 0.0043(2) O1A 0.0435(11) 0.154(3) 0.0573(14) -0.0032(15) 0.0199(11) 0.0093(14) O2A 0.056(4) 0.044(4) 0.096(7) -0.035(3) 0.001(4) 0.007(2) O2B 0.075(7) 0.101(11) 0.028(5) -0.017(5) 0.025(4) 0.020(7) O3A 0.066(4) 0.086(5) 0.040(5) -0.013(4) -0.014(3) 0.005(3) O3B 0.050(6) 0.176(19) 0.033(6) 0.028(8) 0.012(5) 0.041(8) O4A 0.111(6) 0.062(5) 0.085(5) 0.035(4) 0.004(4) -0.011(4) O4B 0.220(17) 0.028(4) 0.135(18) 0.008(6) 0.002(12) -0.049(6) O1W 0.0574(12) 0.0403(10) 0.0364(10) -0.0024(8) 0.0106(9) -0.0037(9) _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 O11 1.8983(13) . ? Co1 O21 1.9137(13) . ? Co1 N21 1.9681(17) . ? Co1 N12 1.9782(18) . ? Co1 N11 1.9820(18) . ? Co1 N22 1.9824(17) . ? Co1 P2 2.7233(5) . ? Co1 P1 2.7326(5) . ? P1 O12 1.4817(15) . ? P1 O11 1.5464(14) . ? P1 C12 1.815(2) . ? P1 C11 1.818(2) . ? C11 N11 1.492(3) . ? C11 H111 0.94(3) . ? C11 H112 0.97(3) . ? N11 H113 0.87(3) . ? N11 H114 0.78(3) . ? C12 N12 1.488(3) . ? C12 H121 1.01(3) . ? C12 H122 0.92(3) . ? N12 H123 0.81(3) . ? N12 H124 0.91(3) . ? P2 O22 1.4919(14) . ? P2 O21 1.5409(14) . ? P2 C21 1.809(2) . ? P2 C22 1.815(2) . ? C21 N21 1.483(3) . ? C21 H211 0.92(3) . ? C21 H212 0.95(3) . ? N21 H213 0.80(3) . ? N21 H214 0.85(3) . ? C22 N22 1.495(3) . ? C22 H221 0.92(3) . ? C22 H222 1.00(3) . ? N22 H223 0.85(3) . ? N22 H224 0.88(3) . ? Cl1 O4B 1.284(16) . ? Cl1 O3A 1.397(13) . ? Cl1 O2B 1.398(13) . ? Cl1 O1A 1.424(2) . ? Cl1 O2A 1.428(10) . ? Cl1 O3B 1.45(2) . ? Cl1 O4A 1.468(10) . ? O4A O4B 0.51(5) . ? O1W H1W1 0.64(4) . ? O1W H1W2 0.86(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 O11 Co1 O21 178.89(6) . . ? O11 Co1 N21 88.74(7) . . ? O21 Co1 N21 90.38(6) . . ? O11 Co1 N12 89.64(7) . . ? O21 Co1 N12 89.72(7) . . ? N21 Co1 N12 92.41(8) . . ? O11 Co1 N11 88.37(7) . . ? O21 Co1 N11 92.50(7) . . ? N21 Co1 N11 177.08(7) . . ? N12 Co1 N11 87.13(8) . . ? O11 Co1 N22 92.30(7) . . ? O21 Co1 N22 88.33(6) . . ? N21 Co1 N22 86.92(8) . . ? N12 Co1 N22 177.93(7) . . ? N11 Co1 N22 93.63(8) . . ? O11 Co1 P2 146.39(4) . . ? O21 Co1 P2 33.38(4) . . ? N21 Co1 P2 65.75(5) . . ? N12 Co1 P2 111.89(5) . . ? N11 Co1 P2 117.08(5) . . ? N22 Co1 P2 66.06(5) . . ? O11 Co1 P1 33.22(4) . . ? O21 Co1 P1 146.88(4) . . ? N21 Co1 P1 111.23(5) . . ? N12 Co1 P1 65.47(5) . . ? N11 Co1 P1 65.97(5) . . ? N22 Co1 P1 116.59(5) . . ? P2 Co1 P1 176.228(18) . . ? O12 P1 O11 116.70(8) . . ? O12 P1 C12 114.82(10) . . ? O11 P1 C12 101.82(9) . . ? O12 P1 C11 116.17(10) . . ? O11 P1 C11 101.98(9) . . ? C12 P1 C11 103.25(11) . . ? O12 P1 Co1 158.95(7) . . ? O11 P1 Co1 42.26(5) . . ? C12 P1 Co1 75.96(7) . . ? C11 P1 Co1 76.12(7) . . ? P1 O11 Co1 104.52(7) . . ? N11 C11 P1 105.52(14) . . ? N11 C11 H111 108.9(16) . . ? P1 C11 H111 110.8(16) . . ? N11 C11 H112 111.7(15) . . ? P1 C11 H112 112.0(16) . . ? H111 C11 H112 108(2) . . ? C11 N11 Co1 112.21(13) . . ? C11 N11 H113 108.0(17) . . ? Co1 N11 H113 108.0(18) . . ? C11 N11 H114 110(2) . . ? Co1 N11 H114 108(2) . . ? H113 N11 H114 111(3) . . ? N12 C12 P1 104.86(13) . . ? N12 C12 H121 109.1(15) . . ? P1 C12 H121 108.8(14) . . ? N12 C12 H122 109.9(17) . . ? P1 C12 H122 111.5(18) . . ? H121 C12 H122 112(2) . . ? C12 N12 Co1 112.23(13) . . ? C12 N12 H123 112(2) . . ? Co1 N12 H123 104(2) . . ? C12 N12 H124 105.9(19) . . ? Co1 N12 H124 112.7(19) . . ? H123 N12 H124 110(3) . . ? O22 P2 O21 116.82(8) . . ? O22 P2 C21 115.17(10) . . ? O21 P2 C21 101.88(10) . . ? O22 P2 C22 115.11(10) . . ? O21 P2 C22 102.87(9) . . ? C21 P2 C22 103.02(11) . . ? O22 P2 Co1 159.91(7) . . ? O21 P2 Co1 43.09(5) . . ? C21 P2 Co1 75.47(7) . . ? C22 P2 Co1 76.43(7) . . ? P2 O21 Co1 103.53(7) . . ? N21 C21 P2 105.29(14) . . ? N21 C21 H211 110.7(19) . . ? P2 C21 H211 109.2(19) . . ? N21 C21 H212 111.7(17) . . ? P2 C21 H212 110.6(18) . . ? H211 C21 H212 109(3) . . ? C21 N21 Co1 111.53(13) . . ? C21 N21 H213 109.2(19) . . ? Co1 N21 H213 109.3(19) . . ? C21 N21 H214 108.5(17) . . ? Co1 N21 H214 111.1(18) . . ? H213 N21 H214 107(3) . . ? N22 C22 P2 105.36(13) . . ? N22 C22 H221 110.3(16) . . ? P2 C22 H221 110.9(16) . . ? N22 C22 H222 107.1(15) . . ? P2 C22 H222 109.2(14) . . ? H221 C22 H222 114(2) . . ? C22 N22 Co1 112.07(12) . . ? C22 N22 H223 108.1(18) . . ? Co1 N22 H223 112.1(18) . . ? C22 N22 H224 105.6(19) . . ? Co1 N22 H224 110.7(19) . . ? H223 N22 H224 108(3) . . ? O4B Cl1 O3A 96.9(13) . . ? O4B Cl1 O2B 113.0(17) . . ? O3A Cl1 O2B 116.0(10) . . ? O4B Cl1 O1A 104.2(14) . . ? O3A Cl1 O1A 113.0(6) . . ? O2B Cl1 O1A 112.2(9) . . ? O4B Cl1 O2A 126.2(17) . . ? O3A Cl1 O2A 111.7(7) . . ? O2B Cl1 O2A 13.2(11) . . ? O1A Cl1 O2A 104.8(6) . . ? O4B Cl1 O3B 112.3(12) . . ? O3A Cl1 O3B 15.5(17) . . ? O2B Cl1 O3B 107.9(12) . . ? O1A Cl1 O3B 107.1(8) . . ? O2A Cl1 O3B 100.9(11) . . ? O4B Cl1 O4A 20(2) . . ? O3A Cl1 O4A 108.4(7) . . ? O2B Cl1 O4A 92.9(9) . . ? O1A Cl1 O4A 112.6(5) . . ? O2A Cl1 O4A 106.0(7) . . ? O3B Cl1 O4A 123.2(14) . . ? O4B O4A Cl1 59(2) . . ? O4A O4B Cl1 100(3) . . ? H1W1 O1W H1W2 109(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.606 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.074 data_cu5end _database_code_CSD 211310 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Cu(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Cu(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety (Cu((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_sum 'C4 H24 Cl4 Cu N4 O6 P2' _chemical_formula_weight 491.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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_Int_Tables_number 14 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 8.1620(2) _cell_length_b 8.0250(2) _cell_length_c 13.3400(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.2850(13) _cell_angle_gamma 90.00 _cell_volume 846.75(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.48 _exptl_crystal_description irregular _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.4mm _exptl_crystal_size_mid 0.35mm _exptl_crystal_size_min 0.2mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 502 _exptl_absorpt_coefficient_mu 2.137 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3718 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1933 _reflns_number_gt 1814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0351P)^2^+0.3536P] 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 SHELXL _refine_ls_extinction_coef 0.067(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1933 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Cu Cu 0.0000 0.0000 0.0000 0.00944(11) Uani 1 2 d S . . Cl1 Cl -0.22875(4) 0.01436(4) 0.07639(3) 0.01387(12) Uani 1 1 d . . . O3W O 0.02721(13) 0.29534(14) 0.01154(8) 0.0161(2) Uani 1 1 d . . . H2W H 0.091(3) 0.344(3) -0.0279(17) 0.049(6) Uiso 1 1 d . . . H1W H 0.040(3) 0.354(3) 0.0696(18) 0.052(7) Uiso 1 1 d . . . P P 0.32350(5) -0.01045(4) 0.20472(3) 0.00820(12) Uani 1 1 d . . . O1 O 0.14572(11) -0.04101(13) 0.13944(7) 0.0114(2) Uani 1 1 d . . . O2 O 0.34018(14) 0.01146(11) 0.31837(8) 0.0131(2) Uani 1 1 d . . . C1 C 0.41130(17) 0.17326(17) 0.15629(10) 0.0121(3) Uani 1 1 d . . . H11 H 0.549(2) -0.151(2) 0.1744(12) 0.016(4) Uiso 1 1 d . . . H12 H 0.471(2) -0.259(2) 0.2457(13) 0.020(4) Uiso 1 1 d . . . C2 C 0.45317(17) -0.18798(17) 0.18609(11) 0.0125(3) Uani 1 1 d . . . H21 H 0.463(2) 0.143(2) 0.1032(13) 0.018(4) Uiso 1 1 d . . . H22 H 0.317(2) 0.251(2) 0.1329(12) 0.017(4) Uiso 1 1 d . . . N1 N 0.37053(15) -0.29204(15) 0.09541(9) 0.0127(2) Uani 1 1 d . . . H11N H 0.327(3) -0.231(3) 0.0380(16) 0.035(5) Uiso 1 1 d . . . H12N H 0.448(2) -0.364(2) 0.0792(13) 0.022(4) Uiso 1 1 d . . . H13N H 0.286(2) -0.350(2) 0.1137(13) 0.020(4) Uiso 1 1 d . . . N2 N 0.54184(15) 0.25795(15) 0.23859(9) 0.0130(2) Uani 1 1 d . . . H21N H 0.621(3) 0.184(3) 0.2783(15) 0.034(5) Uiso 1 1 d . . . H22N H 0.491(2) 0.312(2) 0.2865(14) 0.026(5) Uiso 1 1 d . . . H23N H 0.598(2) 0.329(2) 0.2091(14) 0.026(5) Uiso 1 1 d . . . Cl2 Cl 0.71197(5) 0.50978(4) 0.11162(3) 0.01343(12) 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 Cu 0.00571(16) 0.01373(16) 0.00884(16) 0.00131(7) 0.00171(10) 0.00087(7) Cl1 0.00954(19) 0.0188(2) 0.01436(19) 0.00384(11) 0.00506(15) 0.00275(11) O3W 0.0197(5) 0.0137(5) 0.0150(5) -0.0012(4) 0.0046(4) -0.0019(4) P 0.0061(2) 0.00909(19) 0.0096(2) -0.00003(10) 0.00238(15) 0.00034(10) O1 0.0078(5) 0.0145(4) 0.0114(4) 0.0008(4) 0.0015(4) -0.0007(4) O2 0.0120(5) 0.0169(5) 0.0105(5) -0.0006(3) 0.0030(4) 0.0010(3) C1 0.0107(6) 0.0118(6) 0.0136(6) -0.0001(5) 0.0023(5) -0.0016(5) C2 0.0099(6) 0.0114(6) 0.0159(6) -0.0010(5) 0.0023(5) 0.0003(5) N1 0.0130(6) 0.0116(5) 0.0139(5) -0.0017(4) 0.0041(4) 0.0017(5) N2 0.0107(5) 0.0122(5) 0.0156(5) 0.0008(4) 0.0023(5) -0.0025(5) Cl2 0.0109(2) 0.01395(19) 0.01587(19) -0.00184(10) 0.00403(14) -0.00111(10) _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 Cu O1 1.9727(9) 3 ? Cu O1 1.9727(9) . ? Cu Cl1 2.3402(4) . ? Cu Cl1 2.3402(4) 3 ? Cu O3W 2.3820(11) . ? Cu O3W 2.3820(11) 3 ? O3W H2W 0.91(2) . ? O3W H1W 0.89(2) . ? P O2 1.4986(11) . ? P O1 1.5167(9) . ? P C1 1.8256(14) . ? P C2 1.8280(14) . ? C1 N2 1.4917(17) . ? C1 H21 0.944(17) . ? C1 H22 0.984(18) . ? C2 N1 1.4877(17) . ? C2 H11 0.888(17) . ? C2 H12 0.959(18) . ? N1 H11N 0.90(2) . ? N1 H12N 0.921(19) . ? N1 H13N 0.911(19) . ? N2 H21N 0.94(2) . ? N2 H22N 0.95(2) . ? N2 H23N 0.89(2) . ? 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 Cu O1 180.00(8) 3 . ? O1 Cu Cl1 92.42(3) 3 . ? O1 Cu Cl1 87.58(3) . . ? O1 Cu Cl1 87.58(3) 3 3 ? O1 Cu Cl1 92.42(3) . 3 ? Cl1 Cu Cl1 180.00(2) . 3 ? O1 Cu O3W 85.40(4) 3 . ? O1 Cu O3W 94.60(4) . . ? Cl1 Cu O3W 89.69(3) . . ? Cl1 Cu O3W 90.31(3) 3 . ? O1 Cu O3W 94.60(4) 3 3 ? O1 Cu O3W 85.40(4) . 3 ? Cl1 Cu O3W 90.31(3) . 3 ? Cl1 Cu O3W 89.69(3) 3 3 ? O3W Cu O3W 180.0 . 3 ? Cu O3W H2W 116.4(15) . . ? Cu O3W H1W 124.8(15) . . ? H2W O3W H1W 108(2) . . ? O2 P O1 115.79(6) . . ? O2 P C1 108.52(6) . . ? O1 P C1 109.32(6) . . ? O2 P C2 108.53(6) . . ? O1 P C2 107.45(6) . . ? C1 P C2 106.87(7) . . ? P O1 Cu 141.56(6) . . ? N2 C1 P 112.27(9) . . ? N2 C1 H21 107.3(10) . . ? P C1 H21 110.2(10) . . ? N2 C1 H22 107.8(10) . . ? P C1 H22 106.3(10) . . ? H21 C1 H22 113.0(14) . . ? N1 C2 P 112.74(9) . . ? N1 C2 H11 106.8(11) . . ? P C2 H11 109.1(11) . . ? N1 C2 H12 106.7(11) . . ? P C2 H12 109.0(11) . . ? H11 C2 H12 112.6(15) . . ? C2 N1 H11N 113.0(13) . . ? C2 N1 H12N 110.1(11) . . ? H11N N1 H12N 106.6(16) . . ? C2 N1 H13N 106.9(11) . . ? H11N N1 H13N 109.9(17) . . ? H12N N1 H13N 110.4(16) . . ? C1 N2 H21N 113.3(12) . . ? C1 N2 H22N 110.5(11) . . ? H21N N2 H22N 105.3(15) . . ? C1 N2 H23N 108.8(12) . . ? H21N N2 H23N 107.4(17) . . ? H22N N2 H23N 111.5(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.479 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.071 data_pcl5end _database_code_CSD 211311 _audit_creation_method SHELXL-97 _chemical_name_systematic ; HL*HCl (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'HL*HCl (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H10 Cl N2 O2 P' _chemical_formula_weight 160.54 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' Cl Cl 0.1484 0.1585 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 4.9780(2) _cell_length_b 7.6100(3) _cell_length_c 8.3910(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.750(3) _cell_angle_gamma 90.00 _cell_volume 316.78(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 'all data' _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3mm _exptl_crystal_size_mid 0.2mm _exptl_crystal_size_min 0.2mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 168 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1442 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1442 _reflns_number_gt 1354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0211P)^2^+0.1474P] 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 SHELXL _refine_ls_extinction_coef 0.033(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(8) _refine_ls_number_reflns 1442 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 P P 0.44697(8) 0.79376(11) 0.09704(5) 0.00962(14) Uani 1 1 d . . . O2 O 0.2803(2) 0.7768(2) -0.05926(14) 0.0128(3) Uani 1 1 d . . . O1 O 0.7478(3) 0.8105(2) 0.09440(15) 0.0134(3) Uani 1 1 d . . . N1 N 0.5437(4) 1.0741(3) 0.3035(2) 0.0130(4) Uani 1 1 d . . . H11N H 0.468(6) 1.156(4) 0.373(3) 0.027(7) Uiso 1 1 d . . . H12N H 0.669(6) 0.995(4) 0.368(3) 0.031(7) Uiso 1 1 d . . . H13N H 0.631(5) 1.138(4) 0.241(3) 0.026(7) Uiso 1 1 d . . . N2 N 0.1054(4) 0.5305(3) 0.1794(2) 0.0135(4) Uani 1 1 d . . . H21N H 0.054(7) 0.466(5) 0.273(4) 0.050(9) Uiso 1 1 d . . . H22N H 0.116(5) 0.466(4) 0.094(3) 0.021(7) Uiso 1 1 d . . . H23N H -0.024(6) 0.619(4) 0.152(4) 0.037(8) Uiso 1 1 d . . . C1 C 0.3225(4) 0.9816(3) 0.2060(3) 0.0121(5) Uani 1 1 d . . . H11 H 0.192(4) 0.940(3) 0.277(3) 0.007(5) Uiso 1 1 d . . . H12 H 0.236(4) 1.061(3) 0.137(3) 0.009(5) Uiso 1 1 d . . . C2 C 0.3774(5) 0.6051(3) 0.2225(3) 0.0134(5) Uani 1 1 d . . . H21 H 0.383(4) 0.643(3) 0.331(3) 0.009(6) Uiso 1 1 d . . . H22 H 0.498(5) 0.517(4) 0.205(3) 0.026(7) Uiso 1 1 d . . . Cl Cl 0.89206(8) 0.7849 0.51541(5) 0.01541(14) 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 P 0.0096(2) 0.0088(2) 0.0106(2) 0.0006(2) 0.00186(15) 0.0001(3) O2 0.0130(6) 0.0142(8) 0.0109(6) -0.0012(7) -0.0001(5) 0.0013(8) O1 0.0111(6) 0.0134(8) 0.0160(6) 0.0000(7) 0.0027(5) 0.0008(6) N1 0.0148(9) 0.0110(9) 0.0130(9) -0.0019(7) 0.0009(7) 0.0004(7) N2 0.0117(8) 0.0130(9) 0.0156(9) -0.0001(8) 0.0006(7) -0.0015(7) C1 0.0123(12) 0.0113(12) 0.0127(11) -0.0003(9) 0.0018(9) -0.0006(8) C2 0.0120(10) 0.0130(12) 0.0150(11) -0.0004(9) -0.0002(9) -0.0015(9) Cl 0.0189(2) 0.0136(3) 0.0139(2) 0.0009(2) 0.00244(16) -0.0002(3) _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 P O2 1.4983(12) . ? P O1 1.5050(13) . ? P C2 1.830(2) . ? P C1 1.832(3) . ? N1 C1 1.493(3) . ? N1 H11N 0.95(3) . ? N1 H12N 0.99(3) . ? N1 H13N 0.86(3) . ? N2 C2 1.485(3) . ? N2 H21N 0.98(4) . ? N2 H22N 0.88(3) . ? N2 H23N 0.95(3) . ? C1 H11 0.97(2) . ? C1 H12 0.92(3) . ? C2 H21 0.95(2) . ? C2 H22 0.92(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 P O1 118.29(7) . . ? O2 P C2 108.58(10) . . ? O1 P C2 108.11(11) . . ? O2 P C1 108.56(10) . . ? O1 P C1 108.61(10) . . ? C2 P C1 103.72(10) . . ? C1 N1 H11N 109.3(16) . . ? C1 N1 H12N 114.5(16) . . ? H11N N1 H12N 109(2) . . ? C1 N1 H13N 108.5(17) . . ? H11N N1 H13N 105(3) . . ? H12N N1 H13N 110(2) . . ? C2 N2 H21N 107(2) . . ? C2 N2 H22N 107.5(17) . . ? H21N N2 H22N 115(3) . . ? C2 N2 H23N 112.0(18) . . ? H21N N2 H23N 109(3) . . ? H22N N2 H23N 107(2) . . ? N1 C1 P 112.15(15) . . ? N1 C1 H11 108.4(13) . . ? P C1 H11 109.1(14) . . ? N1 C1 H12 108.5(15) . . ? P C1 H12 111.3(15) . . ? H11 C1 H12 107.2(19) . . ? N2 C2 P 111.83(17) . . ? N2 C2 H21 107.5(14) . . ? P C2 H21 108.6(14) . . ? N2 C2 H22 106.2(17) . . ? P C2 H22 108.9(17) . . ? H21 C2 H22 114(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.286 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.056 data_m6end _database_code_CSD 211312 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Mn(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Mn(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety (Mn((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_sum 'C4 H24 Cl4 Mn N4 O6 P2' _chemical_formula_weight 482.95 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_Int_Tables_number 14 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 8.3320(4) _cell_length_b 7.9230(4) _cell_length_c 13.3980(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.325(4) _cell_angle_gamma 90.00 _cell_volume 860.65(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 28.33 _exptl_crystal_description irregular _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 1.600 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5048 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2038 _reflns_number_gt 1852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0400P)^2^+0.1402P] 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 SHELXL _refine_ls_extinction_coef 0.064(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2038 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _refine_ls_shift/su_max 0.000 _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 Mn Mn 0.5000 0.5000 0.5000 0.01787(14) Uani 1 2 d S . . Cl1 Cl 0.74188(6) 0.48244(5) 0.41732(4) 0.02755(15) Uani 1 1 d . . . O3W O 0.47020(17) 0.22140(16) 0.48897(10) 0.0303(3) Uani 1 1 d . . . H1W H 0.407(6) 0.164(6) 0.540(3) 0.152(18) Uiso 1 1 d . . . H2W H 0.466(4) 0.159(5) 0.431(3) 0.100(12) Uiso 1 1 d . . . P P 0.17233(5) 0.51096(4) 0.28533(3) 0.01537(14) Uani 1 1 d . . . O1 O 0.34482(13) 0.54068(14) 0.34848(9) 0.0207(2) Uani 1 1 d . . . O2 O 0.15234(16) 0.48637(13) 0.17226(10) 0.0244(3) Uani 1 1 d . . . C1 C 0.04533(19) 0.69050(19) 0.30525(13) 0.0217(3) Uani 1 1 d . . . H11 H -0.053(3) 0.655(3) 0.3110(16) 0.033(5) Uiso 1 1 d . . . H12 H 0.040(2) 0.766(3) 0.2460(16) 0.029(5) Uiso 1 1 d . . . C2 C 0.08781(18) 0.32755(18) 0.33845(12) 0.0197(3) Uani 1 1 d . . . H21 H 0.046(3) 0.358(2) 0.3966(17) 0.034(5) Uiso 1 1 d . . . H22 H 0.177(3) 0.249(3) 0.3584(16) 0.033(5) Uiso 1 1 d . . . N1 N 0.11653(18) 0.78495(18) 0.40075(11) 0.0247(3) Uani 1 1 d . . . H11N H 0.149(3) 0.719(3) 0.4560(18) 0.044(6) Uiso 1 1 d . . . H12N H 0.203(3) 0.850(3) 0.3893(17) 0.036(6) Uiso 1 1 d . . . H13N H 0.039(3) 0.845(3) 0.4152(18) 0.045(6) Uiso 1 1 d . . . N2 N -0.04759(17) 0.24445(17) 0.26309(11) 0.0240(3) Uani 1 1 d . . . H21N H -0.124(3) 0.318(3) 0.2223(19) 0.050(7) Uiso 1 1 d . . . H22N H -0.002(3) 0.183(3) 0.2146(18) 0.045(6) Uiso 1 1 d . . . H23N H -0.107(3) 0.175(3) 0.2978(18) 0.045(6) Uiso 1 1 d . . . Cl2 Cl 0.71407(6) 0.48914(5) 0.10576(4) 0.02687(15) 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 Mn 0.0164(2) 0.0203(2) 0.0169(2) 0.00216(10) 0.00372(15) 0.00177(10) Cl1 0.0240(2) 0.0342(2) 0.0276(3) 0.00761(14) 0.01249(18) 0.00703(14) O3W 0.0449(7) 0.0214(6) 0.0248(6) -0.0014(4) 0.0082(5) -0.0016(5) P 0.0140(2) 0.0160(2) 0.0166(3) 0.00054(12) 0.00453(16) 0.00041(11) O1 0.0165(5) 0.0242(5) 0.0207(6) 0.0025(4) 0.0029(4) -0.0007(4) O2 0.0260(6) 0.0295(6) 0.0179(6) -0.0004(4) 0.0056(5) 0.0003(4) C1 0.0181(7) 0.0196(7) 0.0268(8) 0.0012(6) 0.0041(6) 0.0026(5) C2 0.0214(7) 0.0173(6) 0.0206(8) 0.0011(6) 0.0054(6) -0.0012(5) N1 0.0290(7) 0.0224(6) 0.0242(7) -0.0004(5) 0.0092(6) 0.0070(6) N2 0.0230(6) 0.0205(6) 0.0276(7) 0.0007(6) 0.0040(6) -0.0049(5) Cl2 0.0253(3) 0.0251(2) 0.0303(3) 0.00323(14) 0.00655(18) 0.00229(13) _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 Mn O1 2.1649(11) 3_666 ? Mn O1 2.1649(11) . ? Mn O3W 2.2224(13) . ? Mn O3W 2.2224(13) 3_666 ? Mn Cl1 2.5173(5) . ? Mn Cl1 2.5173(5) 3_666 ? O3W H1W 1.06(5) . ? O3W H2W 0.91(4) . ? P O2 1.4982(13) . ? P O1 1.5087(11) . ? P C1 1.8287(15) . ? P C2 1.8290(15) . ? C1 N1 1.483(2) . ? C1 H11 0.88(2) . ? C1 H12 0.99(2) . ? C2 N2 1.4835(19) . ? C2 H21 0.96(2) . ? C2 H22 0.96(2) . ? N1 H11N 0.89(2) . ? N1 H12N 0.93(2) . ? N1 H13N 0.86(3) . ? N2 H21N 0.94(3) . ? N2 H22N 0.96(2) . ? N2 H23N 0.94(2) . ? 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 Mn O1 180.0 3_666 . ? O1 Mn O3W 87.01(5) 3_666 . ? O1 Mn O3W 92.99(5) . . ? O1 Mn O3W 92.99(5) 3_666 3_666 ? O1 Mn O3W 87.01(5) . 3_666 ? O3W Mn O3W 180.00(7) . 3_666 ? O1 Mn Cl1 92.22(3) 3_666 . ? O1 Mn Cl1 87.78(3) . . ? O3W Mn Cl1 90.25(4) . . ? O3W Mn Cl1 89.75(4) 3_666 . ? O1 Mn Cl1 87.78(3) 3_666 3_666 ? O1 Mn Cl1 92.22(3) . 3_666 ? O3W Mn Cl1 89.75(4) . 3_666 ? O3W Mn Cl1 90.25(4) 3_666 3_666 ? Cl1 Mn Cl1 180.0 . 3_666 ? Mn O3W H1W 117(3) . . ? Mn O3W H2W 125(2) . . ? H1W O3W H2W 113(3) . . ? O2 P O1 117.19(7) . . ? O2 P C1 108.39(7) . . ? O1 P C1 107.77(7) . . ? O2 P C2 109.09(7) . . ? O1 P C2 107.95(7) . . ? C1 P C2 105.88(8) . . ? P O1 Mn 142.04(7) . . ? N1 C1 P 112.86(10) . . ? N1 C1 H11 106.3(14) . . ? P C1 H11 109.8(13) . . ? N1 C1 H12 108.8(12) . . ? P C1 H12 105.9(12) . . ? H11 C1 H12 113.2(18) . . ? N2 C2 P 112.85(11) . . ? N2 C2 H21 107.7(12) . . ? P C2 H21 111.3(12) . . ? N2 C2 H22 108.6(12) . . ? P C2 H22 106.5(12) . . ? H21 C2 H22 110.0(18) . . ? C1 N1 H11N 113.9(15) . . ? C1 N1 H12N 108.0(14) . . ? H11N N1 H12N 111(2) . . ? C1 N1 H13N 107.6(16) . . ? H11N N1 H13N 104(2) . . ? H12N N1 H13N 112(2) . . ? C2 N2 H21N 115.3(15) . . ? C2 N2 H22N 109.1(14) . . ? H21N N2 H22N 104.2(19) . . ? C2 N2 H23N 109.4(14) . . ? H21N N2 H23N 107(2) . . ? H22N N2 H23N 112.2(19) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.596 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.140 data_n6end _database_code_CSD 211313 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Ni(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Ni(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety (Ni((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_sum 'C4 H24 Cl4 N4 Ni O6 P2' _chemical_formula_weight 486.72 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' Cl Cl 0.1484 0.1585 '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_Int_Tables_number 14 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 8.2110(3) _cell_length_b 7.8530(2) _cell_length_c 13.2350(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.0420(19) _cell_angle_gamma 90.00 _cell_volume 831.39(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 27.53 _exptl_crystal_description irregular _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.5mm _exptl_crystal_size_mid 0.4mm _exptl_crystal_size_min 0.35mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 2.029 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3648 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.53 _reflns_number_total 1910 _reflns_number_gt 1643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0659P)^2^+0.0922P] 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 SHELXL _refine_ls_extinction_coef 0.0045(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1910 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.003 _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 Ni Ni 1.0000 0.5000 0.5000 0.01245(17) Uani 1 2 d S . . Cl1 Cl 1.23325(7) 0.51759(6) 0.41944(4) 0.01725(19) Uani 1 1 d . . . O3W O 1.0263(2) 0.2355(2) 0.51103(12) 0.0183(4) Uani 1 1 d . . . H1W H 1.087(4) 0.185(4) 0.476(2) 0.038(8) Uiso 1 1 d . . . H2W H 1.019(4) 0.187(5) 0.569(3) 0.070(11) Uiso 1 1 d . . . P P 0.67542(7) 0.49118(6) 0.28910(4) 0.01229(19) Uani 1 1 d . . . O1 O 0.85064(17) 0.46090(18) 0.35253(10) 0.0157(3) Uani 1 1 d . . . O2 O 0.6559(2) 0.51382(16) 0.17442(12) 0.0180(4) Uani 1 1 d . . . C1 C 0.5894(3) 0.6767(3) 0.34168(15) 0.0151(4) Uani 1 1 d . . . H11 H 0.546(3) 0.643(3) 0.3996(16) 0.013(5) Uiso 1 1 d . . . H12 H 0.681(3) 0.758(3) 0.3660(16) 0.020(6) Uiso 1 1 d . . . C2 C 0.5452(3) 0.3109(3) 0.30887(16) 0.0168(4) Uani 1 1 d . . . H21 H 0.441(3) 0.358(3) 0.3183(18) 0.027(6) Uiso 1 1 d . . . H22 H 0.542(3) 0.230(3) 0.2453(17) 0.022(6) Uiso 1 1 d . . . N1 N 0.4542(2) 0.7622(2) 0.26338(14) 0.0167(4) Uani 1 1 d . . . H11N H 0.400(3) 0.835(3) 0.299(2) 0.036(7) Uiso 1 1 d . . . H12N H 0.510(3) 0.823(3) 0.2152(17) 0.020(6) Uiso 1 1 d . . . H13N H 0.375(4) 0.680(4) 0.210(2) 0.054(9) Uiso 1 1 d . . . N2 N 0.6204(2) 0.2113(2) 0.40316(14) 0.0172(4) Uani 1 1 d . . . H21N H 0.541(3) 0.143(3) 0.4189(17) 0.019(6) Uiso 1 1 d . . . H22N H 0.651(4) 0.282(4) 0.457(2) 0.049(9) Uiso 1 1 d . . . H23N H 0.706(3) 0.149(3) 0.3857(19) 0.032(7) Uiso 1 1 d . . . Cl2 Cl 0.22087(7) 0.51469(6) 0.10370(4) 0.01782(19) 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 Ni 0.0093(3) 0.0142(3) 0.0129(3) -0.00120(12) 0.00043(18) -0.00089(12) Cl1 0.0126(3) 0.0214(3) 0.0177(3) -0.00344(17) 0.0033(2) -0.00275(17) O3W 0.0198(8) 0.0164(8) 0.0187(8) -0.0002(6) 0.0045(6) 0.0008(6) P 0.0088(3) 0.0139(3) 0.0133(3) -0.00035(17) 0.0007(2) 0.00032(17) O1 0.0111(8) 0.0183(7) 0.0160(7) -0.0013(6) -0.0008(6) 0.0016(6) O2 0.0153(8) 0.0246(8) 0.0129(7) 0.0008(5) 0.0010(6) 0.0021(5) C1 0.0128(10) 0.0151(10) 0.0158(10) 0.0001(8) -0.0001(8) 0.0018(8) C2 0.0118(10) 0.0169(10) 0.0204(11) -0.0007(8) 0.0010(8) -0.0003(8) N1 0.0133(9) 0.0166(8) 0.0185(9) -0.0004(7) 0.0003(7) 0.0026(7) N2 0.0174(9) 0.0158(9) 0.0178(9) -0.0001(7) 0.0028(8) -0.0029(8) Cl2 0.0143(3) 0.0180(3) 0.0197(3) -0.00137(17) 0.0008(2) -0.00222(17) _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 Ni O1 2.0802(13) 3_766 ? Ni O1 2.0802(13) . ? Ni O3W 2.0901(16) . ? Ni O3W 2.0901(16) 3_766 ? Ni Cl1 2.3970(6) 3_766 ? Ni Cl1 2.3970(6) . ? O3W H1W 0.85(3) . ? O3W H2W 0.87(3) . ? P O2 1.5004(16) . ? P O1 1.5120(15) . ? P C1 1.824(2) . ? P C2 1.828(2) . ? C1 N1 1.496(2) . ? C1 H11 0.95(2) . ? C1 H12 0.98(2) . ? C2 N2 1.484(3) . ? C2 H21 0.96(2) . ? C2 H22 1.05(2) . ? N1 H11N 0.91(3) . ? N1 H12N 0.99(2) . ? N1 H13N 1.07(3) . ? N2 H21N 0.90(3) . ? N2 H22N 0.90(3) . ? N2 H23N 0.92(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 O1 Ni O1 180.0 3_766 . ? O1 Ni O3W 92.95(6) 3_766 . ? O1 Ni O3W 87.05(6) . . ? O1 Ni O3W 87.05(6) 3_766 3_766 ? O1 Ni O3W 92.95(6) . 3_766 ? O3W Ni O3W 180.00(9) . 3_766 ? O1 Ni Cl1 87.26(4) 3_766 3_766 ? O1 Ni Cl1 92.74(4) . 3_766 ? O3W Ni Cl1 89.53(4) . 3_766 ? O3W Ni Cl1 90.47(4) 3_766 3_766 ? O1 Ni Cl1 92.74(4) 3_766 . ? O1 Ni Cl1 87.26(4) . . ? O3W Ni Cl1 90.47(4) . . ? O3W Ni Cl1 89.53(4) 3_766 . ? Cl1 Ni Cl1 180.0 3_766 . ? Ni O3W H1W 119.3(19) . . ? Ni O3W H2W 118(2) . . ? H1W O3W H2W 116(3) . . ? O2 P O1 116.82(9) . . ? O2 P C1 109.22(9) . . ? O1 P C1 108.40(9) . . ? O2 P C2 107.71(9) . . ? O1 P C2 108.23(9) . . ? C1 P C2 105.92(10) . . ? P O1 Ni 141.57(9) . . ? N1 C1 P 112.63(13) . . ? N1 C1 H11 109.2(13) . . ? P C1 H11 109.3(13) . . ? N1 C1 H12 109.0(14) . . ? P C1 H12 108.3(13) . . ? H11 C1 H12 108.2(18) . . ? N2 C2 P 112.49(14) . . ? N2 C2 H21 107.7(14) . . ? P C2 H21 106.7(14) . . ? N2 C2 H22 106.5(13) . . ? P C2 H22 105.2(12) . . ? H21 C2 H22 118(2) . . ? C1 N1 H11N 107.3(17) . . ? C1 N1 H12N 106.5(13) . . ? H11N N1 H12N 112(2) . . ? C1 N1 H13N 115.7(16) . . ? H11N N1 H13N 115(2) . . ? H12N N1 H13N 99.7(18) . . ? C2 N2 H21N 108.6(15) . . ? C2 N2 H22N 109.4(19) . . ? H21N N2 H22N 106(2) . . ? C2 N2 H23N 105.3(16) . . ? H21N N2 H23N 112(2) . . ? H22N N2 H23N 116(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.750 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.129 data_v8end _database_code_CSD 211314 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Ni(L-N,N)2(H2O)2)*2H2O (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common '(Ni(L-N,N)2(H2O)2)*2H2O (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H24 N4 Ni O8 P2' _chemical_formula_weight 376.92 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)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0300(11) _cell_length_b 6.3970(10) _cell_length_c 14.353(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.814(9) _cell_angle_gamma 90.00 _cell_volume 712.78(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 25.12 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.4mm _exptl_crystal_size_mid 0.1mm _exptl_crystal_size_min 0.07mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 396 _exptl_absorpt_coefficient_mu 1.624 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1256 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.12 _reflns_number_total 1256 _reflns_number_gt 1014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0926P)^2^+0.5343P] 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 1256 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1410 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 Ni Ni 1.0000 0.0000 1.0000 0.0314(4) Uani 1 2 d S . . P P 1.40945(17) 0.2844(2) 1.09580(9) 0.0328(4) Uani 1 1 d . . . O1 O 1.6033(5) 0.2886(6) 1.1194(3) 0.0422(9) Uani 1 1 d . . . O2 O 1.3178(6) 0.4775(5) 1.1154(3) 0.0436(10) Uani 1 1 d . . . O3 O 1.1545(6) -0.2556(7) 0.9815(4) 0.0447(12) Uani 1 1 d . . . H3A H 1.196(13) -0.321(16) 1.029(7) 0.12(4) Uiso 1 1 d . . . H3B H 1.199(8) -0.243(9) 0.954(5) 0.03(2) Uiso 1 1 d . . . N1 N 1.1561(6) 0.0570(10) 1.1422(3) 0.0403(12) Uani 1 1 d . . . H1A H 1.106(9) 0.183(12) 1.155(5) 0.07(2) Uiso 1 1 d . . . H1B H 1.118(10) -0.018(11) 1.168(5) 0.05(2) Uiso 1 1 d . . . N2 N 1.1406(6) 0.2153(9) 0.9370(4) 0.0382(11) Uani 1 1 d . . . H2A H 1.101(9) 0.184(10) 0.881(5) 0.06(2) Uiso 1 1 d . . . H2B H 1.099(8) 0.331(10) 0.934(4) 0.043(18) Uiso 1 1 d . . . C1 C 1.3439(7) 0.0717(10) 1.1606(4) 0.0391(13) Uani 1 1 d . . . H11 H 1.396(8) -0.043(9) 1.147(4) 0.048(18) Uiso 1 1 d . . . H12 H 1.386(7) 0.090(8) 1.213(4) 0.025(14) Uiso 1 1 d . . . C2 C 1.3308(7) 0.2203(9) 0.9693(4) 0.0364(12) Uani 1 1 d . . . H21 H 1.385(7) 0.304(8) 0.938(3) 0.029(13) Uiso 1 1 d . . . H22 H 1.379(8) 0.066(11) 0.964(4) 0.046(15) Uiso 1 1 d . . . O99 O 1.1404(7) 0.5857(10) 1.2480(4) 0.0633(15) Uani 1 1 d . . . H991 H 1.230(8) 0.674(9) 1.282(4) 0.049(17) Uiso 1 1 d . . . H992 H 1.176(9) 0.540(9) 1.217(5) 0.04(2) 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 Ni 0.0346(6) 0.0392(6) 0.0243(6) 0.0029(3) 0.0146(4) 0.0007(4) P 0.0359(8) 0.0397(8) 0.0259(7) 0.0014(5) 0.0139(6) 0.0004(6) O1 0.041(2) 0.054(2) 0.035(2) 0.0003(17) 0.0161(16) -0.0030(17) O2 0.055(2) 0.046(2) 0.034(2) 0.0017(15) 0.0180(18) 0.0058(17) O3 0.053(3) 0.053(3) 0.038(3) 0.0120(19) 0.029(2) 0.012(2) N1 0.038(3) 0.055(3) 0.030(3) 0.009(2) 0.013(2) -0.007(3) N2 0.041(3) 0.044(3) 0.031(3) 0.003(2) 0.011(2) -0.003(2) C1 0.039(3) 0.052(3) 0.025(3) 0.004(3) 0.008(2) 0.002(3) C2 0.040(3) 0.043(3) 0.031(3) 0.002(2) 0.019(2) -0.004(3) O99 0.049(3) 0.107(4) 0.041(3) -0.017(3) 0.024(2) -0.007(3) _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 Ni O3 2.110(4) 3_757 ? Ni O3 2.110(4) . ? Ni N2 2.124(5) 3_757 ? Ni N2 2.124(5) . ? Ni N1 2.136(5) . ? Ni N1 2.136(5) 3_757 ? P O2 1.501(4) . ? P O1 1.506(4) . ? P C1 1.801(6) . ? P C2 1.810(5) . ? O3 H3A 0.79(10) . ? O3 H3B 0.60(6) . ? N1 C1 1.467(7) . ? N1 H1A 0.94(8) . ? N1 H1B 0.72(8) . ? N2 C2 1.479(7) . ? N2 H2A 0.81(7) . ? N2 H2B 0.81(6) . ? C1 H11 0.89(6) . ? C1 H12 0.75(5) . ? C2 H21 0.88(5) . ? C2 H22 1.07(7) . ? O99 H991 0.95(7) . ? O99 H992 0.65(7) . ? 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 O3 Ni O3 180.000(2) 3_757 . ? O3 Ni N2 93.2(2) 3_757 3_757 ? O3 Ni N2 86.8(2) . 3_757 ? O3 Ni N2 86.8(2) 3_757 . ? O3 Ni N2 93.2(2) . . ? N2 Ni N2 180.000(1) 3_757 . ? O3 Ni N1 88.2(2) 3_757 . ? O3 Ni N1 91.8(2) . . ? N2 Ni N1 87.1(2) 3_757 . ? N2 Ni N1 92.9(2) . . ? O3 Ni N1 91.8(2) 3_757 3_757 ? O3 Ni N1 88.2(2) . 3_757 ? N2 Ni N1 92.9(2) 3_757 3_757 ? N2 Ni N1 87.1(2) . 3_757 ? N1 Ni N1 180.000(2) . 3_757 ? O2 P O1 118.1(2) . . ? O2 P C1 107.6(3) . . ? O1 P C1 108.6(2) . . ? O2 P C2 108.2(2) . . ? O1 P C2 107.8(2) . . ? C1 P C2 105.9(3) . . ? Ni O3 H3A 116(7) . . ? Ni O3 H3B 116(6) . . ? H3A O3 H3B 116(9) . . ? C1 N1 Ni 120.5(4) . . ? C1 N1 H1A 112(4) . . ? Ni N1 H1A 99(4) . . ? C1 N1 H1B 120(6) . . ? Ni N1 H1B 99(6) . . ? H1A N1 H1B 102(7) . . ? C2 N2 Ni 119.9(4) . . ? C2 N2 H2A 115(5) . . ? Ni N2 H2A 98(5) . . ? C2 N2 H2B 112(4) . . ? Ni N2 H2B 111(4) . . ? H2A N2 H2B 97(6) . . ? N1 C1 P 112.2(4) . . ? N1 C1 H11 115(4) . . ? P C1 H11 107(4) . . ? N1 C1 H12 112(4) . . ? P C1 H12 106(4) . . ? H11 C1 H12 103(6) . . ? N2 C2 P 112.8(4) . . ? N2 C2 H21 117(3) . . ? P C2 H21 106(3) . . ? N2 C2 H22 109(3) . . ? P C2 H22 104(3) . . ? H21 C2 H22 107(5) . . ? H991 O99 H992 102(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.986 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.132 data_zn6end _database_code_CSD 211315 _audit_creation_method SHELXL-97 _chemical_name_systematic ; all-trans-(Zn(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH ) ; _chemical_name_common 'all-trans-(Zn(H2L-O)2(H2O)2Cl2)Cl2 (L = (H2NCH2)2P(O)OH )' _chemical_melting_point ? _chemical_formula_moiety (Zn((H3NCH2)2P(O)OH)2(H2O)2Cl2)Cl2 _chemical_formula_sum 'C4 H24 Cl4 N4 O6 P2 Zn' _chemical_formula_weight 493.38 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 P2(1)/n _symmetry_Int_Tables_number 14 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 8.2290(2) _cell_length_b 7.8630(2) _cell_length_c 13.3150(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.0330(15) _cell_angle_gamma 90.00 _cell_volume 839.35(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data' _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 2.318 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3683 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1922 _reflns_number_gt 1803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0189P)^2^+0.5553P] 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 SHELXL _refine_ls_extinction_coef 0.0180(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1922 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _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 Zn Zn 0.0000 0.0000 0.0000 0.00935(9) Uani 1 2 d S . . Cl1 Cl -0.23434(4) 0.01754(4) 0.08019(3) 0.01326(11) Uani 1 1 d . . . O3W O 0.02846(14) 0.27176(14) 0.01082(8) 0.0147(2) Uani 1 1 d . . . H1W H 0.094(3) 0.322(3) -0.0227(17) 0.038(6) Uiso 1 1 d . . . H2W H 0.028(3) 0.329(3) 0.062(2) 0.052(7) Uiso 1 1 d . . . P P 0.32611(4) -0.01204(4) 0.21186(3) 0.00809(11) Uani 1 1 d . . . O1 O 0.15078(12) -0.04114(13) 0.14907(7) 0.0111(2) Uani 1 1 d . . . O2 O 0.34707(13) 0.01021(12) 0.32582(8) 0.0128(2) Uani 1 1 d . . . C1 C 0.45442(17) -0.19231(18) 0.19079(10) 0.0117(3) Uani 1 1 d . . . H11 H 0.556(2) -0.150(2) 0.1847(13) 0.017(4) Uiso 1 1 d . . . H12 H 0.466(2) -0.269(2) 0.2499(13) 0.017(4) Uiso 1 1 d . . . C2 C 0.41170(17) 0.17384(18) 0.15956(10) 0.0111(3) Uani 1 1 d . . . H21 H 0.456(2) 0.140(2) 0.1035(14) 0.021(5) Uiso 1 1 d . . . H22 H 0.321(2) 0.256(3) 0.1405(13) 0.020(4) Uiso 1 1 d . . . N1 N 0.37705(16) -0.29041(16) 0.09658(9) 0.0125(2) Uani 1 1 d . . . H11N H 0.450(2) -0.358(3) 0.0786(14) 0.025(5) Uiso 1 1 d . . . H12N H 0.335(2) -0.222(3) 0.0359(15) 0.030(5) Uiso 1 1 d . . . H13N H 0.291(2) -0.351(2) 0.1102(14) 0.020(5) Uiso 1 1 d . . . N2 N 0.54587(15) 0.25909(16) 0.23703(9) 0.0122(2) Uani 1 1 d . . . H21N H 0.604(2) 0.327(3) 0.2057(15) 0.029(5) Uiso 1 1 d . . . H22N H 0.621(2) 0.185(3) 0.2777(15) 0.029(5) Uiso 1 1 d . . . H23N H 0.495(2) 0.320(3) 0.2826(15) 0.028(5) Uiso 1 1 d . . . Cl2 Cl 0.71726(4) 0.51351(4) 0.10531(3) 0.01332(10) 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 Zn 0.00879(14) 0.01165(14) 0.00784(14) 0.00127(7) 0.00235(9) 0.00084(8) Cl1 0.01165(18) 0.01718(19) 0.01219(18) 0.00368(12) 0.00527(13) 0.00285(12) O3W 0.0213(5) 0.0117(5) 0.0122(5) -0.0006(4) 0.0064(4) -0.0014(4) P 0.00792(19) 0.00902(18) 0.00775(18) 0.00015(12) 0.00268(13) 0.00013(12) O1 0.0096(5) 0.0138(5) 0.0096(4) 0.0011(4) 0.0019(4) -0.0008(4) O2 0.0133(5) 0.0169(6) 0.0086(5) 0.0000(4) 0.0034(4) -0.0002(4) C1 0.0104(6) 0.0114(7) 0.0129(6) -0.0005(5) 0.0021(5) 0.0009(5) C2 0.0122(6) 0.0111(7) 0.0100(6) -0.0003(5) 0.0025(5) -0.0015(5) N1 0.0157(6) 0.0113(6) 0.0116(5) -0.0010(5) 0.0052(5) 0.0023(5) N2 0.0121(6) 0.0117(6) 0.0127(6) 0.0009(5) 0.0027(5) -0.0022(5) Cl2 0.01291(19) 0.01362(18) 0.01357(18) -0.00179(12) 0.00327(13) -0.00164(12) _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 Zn O1 2.1149(9) . ? Zn O1 2.1149(9) 3 ? Zn O3W 2.1509(11) 3 ? Zn O3W 2.1509(11) . ? Zn Cl1 2.4096(3) 3 ? Zn Cl1 2.4096(3) . ? O3W H1W 0.87(2) . ? O3W H2W 0.82(3) . ? P O2 1.4983(10) . ? P O1 1.5130(10) . ? P C1 1.8265(14) . ? P C2 1.8271(14) . ? C1 N1 1.4879(18) . ? C1 H11 0.923(18) . ? C1 H12 0.981(18) . ? C2 N2 1.4895(17) . ? C2 H21 0.940(18) . ? C2 H22 0.973(19) . ? N1 H11N 0.87(2) . ? N1 H12N 0.97(2) . ? N1 H13N 0.90(2) . ? N2 H21N 0.88(2) . ? N2 H22N 0.93(2) . ? N2 H23N 0.94(2) . ? 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 Zn O1 180.00(3) . 3 ? O1 Zn O3W 86.72(4) . 3 ? O1 Zn O3W 93.28(4) 3 3 ? O1 Zn O3W 93.28(4) . . ? O1 Zn O3W 86.72(4) 3 . ? O3W Zn O3W 180.00(6) 3 . ? O1 Zn Cl1 92.77(3) . 3 ? O1 Zn Cl1 87.23(3) 3 3 ? O3W Zn Cl1 89.96(3) 3 3 ? O3W Zn Cl1 90.04(3) . 3 ? O1 Zn Cl1 87.23(3) . . ? O1 Zn Cl1 92.77(3) 3 . ? O3W Zn Cl1 90.04(3) 3 . ? O3W Zn Cl1 89.96(3) . . ? Cl1 Zn Cl1 180.000(13) 3 . ? Zn O3W H1W 119.0(15) . . ? Zn O3W H2W 125.9(18) . . ? H1W O3W H2W 107(2) . . ? O2 P O1 117.06(6) . . ? O2 P C1 107.92(6) . . ? O1 P C1 108.06(6) . . ? O2 P C2 109.05(6) . . ? O1 P C2 108.18(6) . . ? C1 P C2 106.04(7) . . ? P O1 Zn 141.26(6) . . ? N1 C1 P 112.30(9) . . ? N1 C1 H11 109.7(11) . . ? P C1 H11 107.6(11) . . ? N1 C1 H12 107.5(10) . . ? P C1 H12 108.2(10) . . ? H11 C1 H12 111.6(14) . . ? N2 C2 P 112.66(9) . . ? N2 C2 H21 108.6(11) . . ? P C2 H21 109.1(11) . . ? N2 C2 H22 106.7(11) . . ? P C2 H22 106.8(11) . . ? H21 C2 H22 113.1(15) . . ? C1 N1 H11N 110.8(13) . . ? C1 N1 H12N 114.9(12) . . ? H11N N1 H12N 104.4(16) . . ? C1 N1 H13N 108.1(11) . . ? H11N N1 H13N 110.5(18) . . ? H12N N1 H13N 108.1(16) . . ? C2 N2 H21N 110.0(13) . . ? C2 N2 H22N 114.4(13) . . ? H21N N2 H22N 107.2(17) . . ? C2 N2 H23N 108.1(12) . . ? H21N N2 H23N 110.9(18) . . ? H22N N2 H23N 106.1(16) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.401 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.061 data_zp2end _database_code_CSD 211316 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Zn(L)2)*2H2O (L = (H2NCH2)2P(O)OH )? ; _chemical_name_common '(Zn(L)2)*2H2O (L = (H2NCH2)2P(O)OH )?' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H20 N4 O6 P2 Zn' _chemical_formula_weight 347.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.69900(10) _cell_length_b 17.2390(3) _cell_length_c 6.2940(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.3510(15) _cell_angle_gamma 90.00 _cell_volume 618.34(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all data (CCD)' _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 34.99 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4mm _exptl_crystal_size_mid 0.2mm _exptl_crystal_size_min 0.1mm _exptl_crystal_density_meas -- _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 2.268 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13276 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 34.99 _reflns_number_total 2670 _reflns_number_gt 2414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0327P)^2^+0.2042P] 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 SHELXL _refine_ls_extinction_coef 0.045(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2670 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Zn Zn 1.0000 0.0000 1.0000 0.01973(7) Uani 1 2 d S . . P P 0.72960(5) 0.102530(17) 0.67256(4) 0.01802(8) Uani 1 1 d . . . O1 O 0.72744(15) 0.02207(5) 0.76860(14) 0.02254(16) Uani 1 1 d . . . O2 O 0.49416(15) 0.14125(6) 0.63897(15) 0.02729(19) Uani 1 1 d . . . N1 N 1.10693(17) 0.11612(6) 0.93610(17) 0.02138(17) Uani 1 1 d . . . H11N H 1.211(3) 0.1141(11) 0.851(3) 0.031(5) Uiso 1 1 d . . . H12N H 1.166(3) 0.1388(11) 1.043(3) 0.025(4) Uiso 1 1 d . . . C1 C 0.9106(2) 0.16232(7) 0.8469(2) 0.0237(2) Uani 1 1 d . . . H11 H 0.966(4) 0.2045(13) 0.771(4) 0.042(5) Uiso 1 1 d . . . H12 H 0.802(3) 0.1783(12) 0.970(3) 0.035(5) Uiso 1 1 d . . . N2 N 0.77050(18) 0.04384(7) 1.26676(17) 0.0250(2) Uani 1 1 d . . . H21N H 0.726(5) 0.0019(13) 1.337(5) 0.047(7) Uiso 1 1 d . . . H22N H 0.648(4) 0.0605(13) 1.218(4) 0.046(6) Uiso 1 1 d . . . C2 C 0.8811(2) 0.09831(7) 0.41857(18) 0.0219(2) Uani 1 1 d . . . H21 H 0.877(4) 0.1513(13) 0.358(3) 0.041(5) Uiso 1 1 d . . . H22 H 1.037(3) 0.0837(11) 0.441(3) 0.026(4) Uiso 1 1 d . . . O99 O 0.3998(3) 0.20115(8) 1.2392(2) 0.0493(4) Uani 1 1 d . . . H991 H 0.418(4) 0.1913(14) 1.356(4) 0.045(6) Uiso 1 1 d . . . H992 H 0.433(5) 0.2434(16) 1.230(4) 0.055(7) 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 Zn 0.02105(10) 0.02046(11) 0.01764(10) 0.00136(6) -0.00169(6) -0.00104(6) P 0.01749(12) 0.02172(15) 0.01484(12) -0.00046(9) -0.00007(9) 0.00095(9) O1 0.0227(3) 0.0231(4) 0.0217(4) 0.0017(3) -0.0033(3) -0.0041(3) O2 0.0225(4) 0.0367(5) 0.0226(4) 0.0018(3) 0.0001(3) 0.0084(3) N1 0.0201(4) 0.0252(4) 0.0188(4) -0.0022(3) -0.0010(3) -0.0034(3) C1 0.0284(5) 0.0206(5) 0.0221(5) -0.0025(4) -0.0027(4) -0.0001(4) N2 0.0214(4) 0.0339(5) 0.0197(4) -0.0052(4) 0.0010(3) -0.0023(4) C2 0.0221(4) 0.0257(5) 0.0179(4) -0.0015(4) 0.0031(3) -0.0022(4) O99 0.0778(10) 0.0362(6) 0.0335(6) 0.0054(5) -0.0244(6) -0.0154(6) _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 Zn N1 2.1315(10) 3_757 ? Zn N1 2.1315(10) . ? Zn O1 2.1566(9) 3_757 ? Zn O1 2.1566(9) . ? Zn N2 2.2644(10) . ? Zn N2 2.2644(10) 3_757 ? P O2 1.5123(9) . ? P O1 1.5131(10) . ? P C1 1.8213(12) . ? P C2 1.8230(11) . ? N1 C1 1.4809(16) . ? N1 H11N 0.80(2) . ? N1 H12N 0.846(19) . ? C1 H11 0.93(2) . ? C1 H12 1.03(2) . ? N2 C2 1.4782(16) 1_556 ? N2 H21N 0.88(2) . ? N2 H22N 0.81(2) . ? C2 N2 1.4782(16) 1_554 ? C2 H21 0.99(2) . ? C2 H22 0.931(18) . ? O99 H991 0.76(3) . ? O99 H992 0.75(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 N1 Zn N1 180.00(2) 3_757 . ? N1 Zn O1 84.98(4) 3_757 3_757 ? N1 Zn O1 95.02(4) . 3_757 ? N1 Zn O1 95.02(4) 3_757 . ? N1 Zn O1 84.98(4) . . ? O1 Zn O1 180.0 3_757 . ? N1 Zn N2 90.37(4) 3_757 . ? N1 Zn N2 89.63(4) . . ? O1 Zn N2 88.57(4) 3_757 . ? O1 Zn N2 91.43(4) . . ? N1 Zn N2 89.63(4) 3_757 3_757 ? N1 Zn N2 90.37(4) . 3_757 ? O1 Zn N2 91.43(4) 3_757 3_757 ? O1 Zn N2 88.57(4) . 3_757 ? N2 Zn N2 180.0 . 3_757 ? O2 P O1 116.81(5) . . ? O2 P C1 109.47(6) . . ? O1 P C1 106.50(5) . . ? O2 P C2 108.64(5) . . ? O1 P C2 108.59(5) . . ? C1 P C2 106.34(6) . . ? P O1 Zn 115.08(5) . . ? C1 N1 Zn 111.13(7) . . ? C1 N1 H11N 109.2(14) . . ? Zn N1 H11N 107.4(14) . . ? C1 N1 H12N 110.5(12) . . ? Zn N1 H12N 113.4(13) . . ? H11N N1 H12N 105.0(18) . . ? N1 C1 P 110.36(8) . . ? N1 C1 H11 111.1(14) . . ? P C1 H11 109.0(14) . . ? N1 C1 H12 108.4(12) . . ? P C1 H12 105.2(12) . . ? H11 C1 H12 112.6(18) . . ? C2 N2 Zn 116.45(7) 1_556 . ? C2 N2 H21N 108.7(18) 1_556 . ? Zn N2 H21N 105.3(17) . . ? C2 N2 H22N 112.4(17) 1_556 . ? Zn N2 H22N 109.6(16) . . ? H21N N2 H22N 103(2) . . ? N2 C2 P 112.94(8) 1_554 . ? N2 C2 H21 109.2(13) 1_554 . ? P C2 H21 107.0(12) . . ? N2 C2 H22 109.1(11) 1_554 . ? P C2 H22 109.6(12) . . ? H21 C2 H22 108.9(16) . . ? H991 O99 H992 105(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 34.99 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.722 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.086