#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/81/4308149.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4308149 loop_ _publ_author_name 'Sanjit Konar' 'Jerzy Zo\'n' 'Andrey V. Prosvirin' 'Kim R. Dunbar' 'Abraham Clearfield' _publ_section_title ; Synthesis and Characterization of Four Metal-Organophosphonates with One-, Two-, and Three-Dimensional Structures ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 5229 _journal_page_last 5236 _journal_volume 46 _journal_year 2007 _chemical_formula_sum 'C5 H6 Cl2 N O3 P Zn' _chemical_formula_weight 295.34 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.860(11) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.497(5) _cell_length_b 9.391(5) _cell_length_c 12.378(6) _cell_measurement_reflns_used 786 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 0.00 _cell_measurement_theta_min 0.00 _cell_volume 987.6(9) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 4363 _diffrn_reflns_theta_full 23.66 _diffrn_reflns_theta_max 23.66 _diffrn_reflns_theta_min 2.72 _exptl_absorpt_coefficient_mu 3.161 _exptl_absorpt_correction_type 'Bruker SADABS V2.10' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.986 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _refine_diff_density_max 2.416 _refine_diff_density_min -2.295 _refine_diff_density_rms 0.477 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1491 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.128 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0727 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1654P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2028 _refine_ls_wR_factor_ref 0.2135 _reflns_number_gt 1353 _reflns_number_total 1491 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic070132u-file004.cif _[local]_cod_data_source_block Complex_3 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4308149 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' 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 Zn1 Zn 0.13584(8) 0.29604(6) 0.52997(6) 0.0123(5) Uani 1 1 d . . . Cl1 Cl 0.3324(2) 0.30784(14) 0.41543(14) 0.0187(6) Uani 1 1 d . . . P3 P -0.13440(18) 0.40175(14) 0.35600(13) 0.0116(5) Uani 1 1 d . . . Cl2 Cl 0.09503(19) 0.08606(14) 0.61358(12) 0.0178(6) Uani 1 1 d . . . O2 O -0.0704(5) 0.3347(4) 0.4583(4) 0.0155(10) Uani 1 1 d . . . O7 O 0.1503(5) 0.4387(4) 0.6445(3) 0.0167(10) Uani 1 1 d . . . O1 O -0.2926(5) 0.3216(4) 0.3361(4) 0.0173(11) Uani 1 1 d . . . H7 H -0.3322 0.3479 0.2787 0.026 Uiso 1 1 calc R . . C1 C 0.0190(8) 0.2160(6) 0.2162(6) 0.0161(16) Uani 1 1 d . . . H1 H -0.0330 0.1434 0.2523 0.019 Uiso 1 1 calc R . . N1 N 0.1931(7) 0.2911(5) 0.0845(5) 0.0186(14) Uani 1 1 d . . . H2 H 0.2594 0.2702 0.0351 0.022 Uiso 1 1 calc R . . C3 C -0.0066(7) 0.3575(6) 0.2439(5) 0.0116(13) Uani 1 1 d . . . C4 C 0.1203(9) 0.1845(7) 0.1360(6) 0.0225(17) Uani 1 1 d . . . H4 H 0.1392 0.0904 0.1169 0.027 Uiso 1 1 calc R . . C5 C 0.0654(7) 0.4638(6) 0.1860(5) 0.0165(14) Uani 1 1 d . . . H5 H 0.0449 0.5589 0.2011 0.020 Uiso 1 1 calc R . . C6 C 0.1670(8) 0.4278(7) 0.1063(5) 0.0209(16) Uani 1 1 d . . . H6 H 0.2178 0.4984 0.0674 0.025 Uiso 1 1 calc R . . 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 Zn1 0.0259(7) 0.0048(6) 0.0062(7) -0.0003(2) 0.0065(4) 0.0012(2) Cl1 0.0302(11) 0.0103(9) 0.0162(11) -0.0016(6) 0.0139(8) 0.0001(5) P3 0.0248(11) 0.0061(9) 0.0041(10) -0.0001(6) 0.0073(8) 0.0005(6) Cl2 0.0362(10) 0.0070(8) 0.0102(11) 0.0019(5) 0.0032(8) -0.0029(6) O2 0.029(3) 0.0110(19) 0.006(2) 0.0003(18) 0.0039(19) -0.0027(19) O7 0.032(3) 0.010(2) 0.009(2) 0.0012(18) 0.0059(19) 0.0061(18) O1 0.023(3) 0.021(2) 0.008(3) 0.0020(19) 0.003(2) -0.0020(18) C1 0.025(4) 0.008(3) 0.016(4) -0.001(2) 0.007(3) 0.000(2) N1 0.029(3) 0.020(3) 0.007(3) -0.003(2) 0.008(3) 0.001(2) C3 0.026(3) 0.005(3) 0.003(3) 0.000(2) 0.002(3) -0.001(2) C4 0.042(5) 0.009(3) 0.017(4) -0.007(3) 0.009(3) 0.004(3) C5 0.031(4) 0.006(3) 0.013(4) 0.000(2) 0.010(3) 0.002(2) C6 0.030(4) 0.014(3) 0.019(4) 0.005(3) 0.011(3) -0.006(3) 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' Zn Zn 0.2839 1.4301 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O2 104.14(17) . . ? O7 Zn1 Cl1 113.03(13) . . ? O2 Zn1 Cl1 112.00(14) . . ? O7 Zn1 Cl2 105.98(13) . . ? O2 Zn1 Cl2 102.94(13) . . ? Cl1 Zn1 Cl2 117.45(6) . . ? O7 P3 O2 116.8(3) 3_566 . ? O7 P3 O1 113.8(3) 3_566 . ? O2 P3 O1 103.3(3) . . ? O7 P3 C3 106.2(2) 3_566 . ? O2 P3 C3 109.4(3) . . ? O1 P3 C3 107.0(3) . . ? P3 O2 Zn1 139.1(3) . . ? P3 O7 Zn1 132.5(3) 3_566 . ? C4 C1 C3 119.5(6) . . ? C6 N1 C4 122.9(6) . . ? C5 C3 C1 119.5(6) . . ? C5 C3 P3 120.4(4) . . ? C1 C3 P3 120.2(5) . . ? N1 C4 C1 119.2(6) . . ? C6 C5 C3 119.2(5) . . ? N1 C6 C5 119.7(6) . . ? 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 Zn1 O7 1.953(4) . ? Zn1 O2 1.986(5) . ? Zn1 Cl1 2.2095(19) . ? Zn1 Cl2 2.2562(18) . ? P3 O7 1.504(4) 3_566 ? P3 O2 1.508(5) . ? P3 O1 1.557(5) . ? P3 C3 1.822(6) . ? O7 P3 1.504(4) 3_566 ? C1 C4 1.357(10) . ? C1 C3 1.391(8) . ? N1 C6 1.331(8) . ? N1 C4 1.342(8) . ? C3 C5 1.377(8) . ? C5 C6 1.363(8) . ? _journal_paper_doi 10.1021/ic070132u