#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/08/4300837.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_4300837 loop_ _publ_author_name 'John A. Groves' 'Paul A. Wright' 'Philip Lightfoot' _publ_contact_author 'Philip Lightfoot' _publ_contact_author_address ; Dr P. Lightfoot School of Chemistry University of St Andrews St Andrews Fife KY16 9ST UK ; _publ_contact_author_email pl@st-and.ac.uk _publ_section_title ; Two Closely Related Lanthanum Phosphonate Frameworks Formed by Anion-Directed Linking of Inorganic Chains ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1736 _journal_page_last 1739 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C9 H22 Cl La N3 O9 P3' _chemical_formula_weight 583.57 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 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 102.521(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.1071(6) _cell_length_b 21.710(2) _cell_length_c 13.7316(13) _cell_measurement_reflns_used 186 _cell_measurement_temperature 295(2) _cell_volume 1777.3(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 295(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 0.0847 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10645 _diffrn_reflns_theta_full 25.36 _diffrn_reflns_theta_max 25.36 _diffrn_reflns_theta_min 1.79 _exptl_absorpt_coefficient_mu 2.876 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9178 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1152 _exptl_crystal_size_max .3 _exptl_crystal_size_mid .03 _exptl_crystal_size_min .01 _refine_diff_density_max 0.850 _refine_diff_density_min -1.683 _refine_diff_density_rms 0.217 _refine_ls_extinction_coef 0.0019(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 237 _refine_ls_number_reflns 3259 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.250 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0792 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+33.0082P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1264 _refine_ls_wR_factor_ref 0.1340 _reflns_number_gt 2588 _reflns_number_total 3259 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048456vsi20041104_054522_2.cif _[local]_cod_data_source_block (I) _[local]_cod_cif_authors_sg_H-M 'P 1 21/c 1 ' _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 4300837 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' 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 La1 La 0.34031(11) 0.48499(3) 0.62502(5) 0.0109(2) Uani 1 1 d . . . Cl1 Cl 0.2131(6) 0.32672(17) 1.0551(3) 0.0365(9) Uani 1 1 d . . . P1 P -0.1736(5) 0.55863(12) 0.6571(2) 0.0124(6) Uani 1 1 d . . . P2 P -0.2026(5) 0.39320(13) 0.5595(2) 0.0131(6) Uani 1 1 d . . . P3 P 0.6059(5) 0.38540(13) 0.8466(2) 0.0163(7) Uani 1 1 d . . . O1 O -0.2726(13) 0.5316(3) 0.5563(6) 0.0170(18) Uani 1 1 d . . . O2 O 0.0653(12) 0.5401(3) 0.7038(6) 0.0159(17) Uani 1 1 d . . . O3 O -0.3331(13) 0.5476(3) 0.7286(6) 0.0164(17) Uani 1 1 d . . . O4 O 0.0390(12) 0.4098(4) 0.6039(6) 0.0214(19) Uani 1 1 d . . . O5 O -0.2782(13) 0.4094(3) 0.4505(6) 0.0168(17) Uani 1 1 d . . . O6 O -0.3643(14) 0.4100(4) 0.6232(6) 0.0229(19) Uani 1 1 d . . . O7 O 0.4288(12) 0.4293(3) 0.7947(6) 0.0179(18) Uani 1 1 d . . . O8 O 0.5845(15) 0.3763(4) 0.9590(6) 0.025(2) Uani 1 1 d . . . H8 H 0.5695 0.4100 0.9838 0.037 Uiso 1 1 calc R . . O9 O 0.6261(14) 0.3236(4) 0.8024(6) 0.025(2) Uani 1 1 d . . . C1 C -0.187(2) 0.6413(5) 0.6305(9) 0.018(3) Uani 1 1 d . . . H1A H -0.1052 0.6495 0.5788 0.022 Uiso 1 1 calc R . . H1B H -0.3425 0.6525 0.6044 0.022 Uiso 1 1 calc R . . C2 C -0.161(2) 0.7476(5) 0.7012(9) 0.021(3) Uani 1 1 d . . . H2A H -0.3231 0.7499 0.6789 0.025 Uiso 1 1 calc R . . H2B H -0.0952 0.7638 0.6484 0.025 Uiso 1 1 calc R . . C3 C -0.090(2) 0.7866(5) 0.7924(9) 0.017(3) Uani 1 1 d . . . H3A H -0.1723 0.7742 0.8421 0.021 Uiso 1 1 calc R . . H3B H -0.1265 0.8293 0.7755 0.021 Uiso 1 1 calc R . . C4 C 0.2386(19) 0.7152(5) 0.8423(9) 0.018(3) Uani 1 1 d . . . H4A H 0.4013 0.7142 0.8579 0.021 Uiso 1 1 calc R . . H4B H 0.1875 0.6948 0.8962 0.021 Uiso 1 1 calc R . . C5 C 0.154(2) 0.6804(6) 0.7476(9) 0.025(3) Uani 1 1 d . . . H5A H 0.2151 0.6985 0.6945 0.030 Uiso 1 1 calc R . . H5B H 0.2047 0.6380 0.7561 0.030 Uiso 1 1 calc R . . C6 C 0.214(2) 0.8089(5) 0.9385(9) 0.022(3) Uani 1 1 d . . . H6A H 0.3627 0.7959 0.9724 0.026 Uiso 1 1 calc R . . H6B H 0.1084 0.7929 0.9759 0.026 Uiso 1 1 calc R . . C7 C 0.8797(18) 0.4228(5) 0.8667(9) 0.017(3) Uani 1 1 d . . . H7A H 0.9812 0.4007 0.9194 0.021 Uiso 1 1 calc R . . H7B H 0.9365 0.4182 0.8064 0.021 Uiso 1 1 calc R . . C8 C 0.7632(18) 0.5080(5) 0.9732(8) 0.017(2) Uani 1 1 d . . . H8A H 0.7496 0.5525 0.9748 0.021 Uiso 1 1 calc R . . H8B H 0.6131 0.4909 0.9558 0.021 Uiso 1 1 calc R . . C9 C 1.1221(17) 0.5146(6) 0.9247(8) 0.018(2) Uani 1 1 d . . . H9A H 1.1182 0.5593 0.9249 0.022 Uiso 1 1 calc R . . H9B H 1.2079 0.5017 0.8766 0.022 Uiso 1 1 calc R . . N1 N -0.0936(15) 0.6819(4) 0.7195(7) 0.016(2) Uani 1 1 d . . . H1 H -0.1478 0.6681 0.7723 0.019 Uiso 1 1 calc R . . N2 N 0.1613(15) 0.7810(4) 0.8364(7) 0.014(2) Uani 1 1 d . . . H2 H 0.2369 0.8022 0.7969 0.017 Uiso 1 1 calc R . . N3 N 0.8889(14) 0.4905(4) 0.8940(6) 0.0141(19) Uani 1 1 d . . . H3 H 0.8230 0.5113 0.8377 0.017 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 La1 0.0112(3) 0.0122(3) 0.0092(3) -0.0003(3) 0.0018(2) -0.0002(3) Cl1 0.0266(18) 0.041(2) 0.043(2) 0.0164(17) 0.0099(16) 0.0025(15) P1 0.0130(15) 0.0100(13) 0.0137(15) -0.0001(11) 0.0017(13) -0.0007(11) P2 0.0141(15) 0.0104(14) 0.0152(16) 0.0004(12) 0.0044(12) 0.0004(11) P3 0.0147(16) 0.0183(15) 0.0154(16) 0.0017(12) 0.0022(12) -0.0001(12) O1 0.025(4) 0.010(4) 0.014(4) -0.003(3) 0.000(4) -0.003(3) O2 0.016(4) 0.017(4) 0.014(4) 0.000(3) 0.000(3) 0.003(3) O3 0.018(4) 0.021(4) 0.012(4) 0.001(3) 0.008(3) 0.002(3) O4 0.005(4) 0.020(4) 0.037(5) 0.005(4) 0.001(4) -0.007(3) O5 0.022(4) 0.015(4) 0.015(4) 0.003(3) 0.007(4) 0.004(3) O6 0.027(5) 0.020(4) 0.024(5) 0.004(4) 0.011(4) 0.007(4) O7 0.014(4) 0.022(4) 0.019(4) 0.003(3) 0.004(4) 0.001(3) O8 0.034(5) 0.026(5) 0.017(5) 0.006(4) 0.009(4) 0.004(4) O9 0.033(5) 0.016(4) 0.027(5) -0.003(4) 0.013(4) -0.004(4) C1 0.021(7) 0.018(6) 0.013(6) -0.009(5) -0.002(5) -0.002(5) C2 0.023(7) 0.015(6) 0.024(7) 0.006(5) 0.006(6) 0.006(5) C3 0.024(6) 0.017(6) 0.013(6) -0.001(5) 0.007(5) 0.006(5) C4 0.016(6) 0.008(5) 0.030(7) 0.008(5) 0.006(5) -0.002(4) C5 0.025(7) 0.025(7) 0.022(7) -0.003(6) 0.001(6) 0.004(6) C6 0.020(6) 0.020(6) 0.019(7) 0.002(5) -0.007(5) -0.003(5) C7 0.015(6) 0.011(5) 0.027(7) -0.006(5) 0.006(5) 0.002(5) C8 0.011(5) 0.019(6) 0.020(6) -0.005(5) -0.001(5) 0.000(5) C9 0.010(5) 0.029(6) 0.013(6) 0.000(6) -0.003(4) 0.003(5) N1 0.019(5) 0.009(4) 0.022(6) 0.007(4) 0.008(4) 0.003(4) N2 0.019(5) 0.014(5) 0.013(5) 0.006(4) 0.011(4) 0.002(4) N3 0.015(5) 0.019(5) 0.008(4) 0.001(4) 0.001(4) -0.005(4) 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' La La -0.2871 2.4523 '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 O4 La1 O6 95.4(3) . 1_655 ? O4 La1 O1 79.9(3) . 3_566 ? O6 La1 O1 81.6(3) 1_655 3_566 ? O4 La1 O2 79.1(3) . . ? O6 La1 O2 153.7(3) 1_655 . ? O1 La1 O2 121.9(3) 3_566 . ? O4 La1 O5 121.4(3) . 3_566 ? O6 La1 O5 130.7(3) 1_655 3_566 ? O1 La1 O5 74.8(2) 3_566 3_566 ? O2 La1 O5 71.6(2) . 3_566 ? O4 La1 O3 153.8(3) . 1_655 ? O6 La1 O3 82.6(3) 1_655 1_655 ? O1 La1 O3 125.2(2) 3_566 1_655 ? O2 La1 O3 91.2(2) . 1_655 ? O5 La1 O3 77.1(2) 3_566 1_655 ? O4 La1 O7 78.3(3) . . ? O6 La1 O7 71.6(3) 1_655 . ? O1 La1 O7 143.4(2) 3_566 . ? O2 La1 O7 82.1(2) . . ? O5 La1 O7 141.7(2) 3_566 . ? O3 La1 O7 76.2(2) 1_655 . ? O4 La1 O1 147.4(3) . 1_655 ? O6 La1 O1 64.7(2) 1_655 1_655 ? O1 La1 O1 72.1(3) 3_566 1_655 ? O2 La1 O1 130.2(2) . 1_655 ? O5 La1 O1 67.0(2) 3_566 1_655 ? O3 La1 O1 53.8(2) 1_655 1_655 ? O7 La1 O1 115.5(2) . 1_655 ? O4 La1 P1 166.61(19) . 1_655 ? O6 La1 P1 71.3(2) 1_655 1_655 ? O1 La1 P1 98.87(19) 3_566 1_655 ? O2 La1 P1 112.26(18) . 1_655 ? O5 La1 P1 70.46(18) 3_566 1_655 ? O3 La1 P1 26.81(17) 1_655 1_655 ? O7 La1 P1 95.72(18) . 1_655 ? O1 La1 P1 26.96(15) 1_655 1_655 ? O1 P1 O2 116.3(5) . . ? O1 P1 O3 109.9(5) . . ? O2 P1 O3 111.9(4) . . ? O1 P1 C1 102.0(5) . . ? O2 P1 C1 110.0(5) . . ? O3 P1 C1 105.8(5) . . ? O1 P1 La1 61.3(3) . 1_455 ? O2 P1 La1 132.9(3) . 1_455 ? O3 P1 La1 48.7(3) . 1_455 ? C1 P1 La1 116.5(4) . 1_455 ? O6 P2 O5 115.0(5) . . ? O6 P2 O4 114.5(5) . . ? O5 P2 O4 113.9(5) . . ? O6 P2 C6 101.7(6) . 2_546 ? O5 P2 C6 104.1(5) . 2_546 ? O4 P2 C6 105.6(5) . 2_546 ? O9 P3 O7 119.6(5) . . ? O9 P3 O8 108.4(5) . . ? O7 P3 O8 109.7(5) . . ? O9 P3 C7 107.9(5) . . ? O7 P3 C7 109.4(5) . . ? O8 P3 C7 100.0(5) . . ? P1 O1 La1 159.1(5) . 3_566 ? P1 O1 La1 91.7(4) . 1_455 ? La1 O1 La1 107.9(3) 3_566 1_455 ? P1 O2 La1 128.4(4) . . ? P1 O3 La1 104.5(4) . 1_455 ? P2 O4 La1 148.8(5) . . ? P2 O5 La1 127.5(4) . 3_566 ? P2 O6 La1 138.8(5) . 1_455 ? P3 O7 La1 135.7(5) . . ? N1 C1 P1 114.6(8) . . ? N1 C2 C3 112.3(10) . . ? C2 C3 N2 111.8(9) . . ? C5 C4 N2 112.8(9) . . ? N1 C5 C4 110.9(10) . . ? N2 C6 P2 114.6(8) . 2_556 ? N3 C7 P3 116.9(7) . . ? C9 C8 N3 112.4(9) 3_767 . ? N3 C9 C8 111.8(9) . 3_767 ? C5 N1 C2 107.2(9) . . ? C5 N1 C1 112.5(9) . . ? C2 N1 C1 112.2(9) . . ? C6 N2 C4 109.5(8) . . ? C6 N2 C3 109.3(9) . . ? C4 N2 C3 112.0(8) . . ? C9 N3 C8 108.1(8) . . ? C9 N3 C7 113.2(9) . . ? C8 N3 C7 115.2(9) . . ? 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 La1 O4 2.429(7) . ? La1 O6 2.434(8) 1_655 ? La1 O1 2.461(8) 3_566 ? La1 O2 2.492(8) . ? La1 O5 2.511(7) 3_566 ? La1 O3 2.572(8) 1_655 ? La1 O7 2.576(8) . ? La1 O1 2.910(8) 1_655 ? La1 P1 3.316(3) 1_655 ? P1 O1 1.504(8) . ? P1 O2 1.515(8) . ? P1 O3 1.545(8) . ? P1 C1 1.829(11) . ? P1 La1 3.316(3) 1_455 ? P2 O6 1.499(9) . ? P2 O5 1.509(8) . ? P2 O4 1.513(8) . ? P2 C6 1.831(12) 2_546 ? P3 O9 1.488(8) . ? P3 O7 1.501(8) . ? P3 O8 1.589(8) . ? P3 C7 1.825(11) . ? O1 La1 2.461(8) 3_566 ? O1 La1 2.910(8) 1_455 ? O3 La1 2.572(8) 1_455 ? O5 La1 2.511(7) 3_566 ? O6 La1 2.434(8) 1_455 ? C1 N1 1.515(14) . ? C2 N1 1.492(13) . ? C2 C3 1.496(16) . ? C3 N2 1.527(14) . ? C4 C5 1.495(16) . ? C4 N2 1.502(13) . ? C5 N1 1.478(15) . ? C6 N2 1.498(15) . ? C6 P2 1.831(12) 2_556 ? C7 N3 1.515(13) . ? C8 C9 1.507(15) 3_767 ? C8 N3 1.509(14) . ? C9 N3 1.490(13) . ? C9 C8 1.507(15) 3_767 ? _journal_paper_doi 10.1021/ic048456v