Three novel coordination polymers based on tris(p-carboxyphenyl)phosphane oxide: Syntheses, structural characterization and magnetic properties
Huo, Liangqin; Fan, Liming; Zhang, Jie; Gao, Lingling; Zhai, Lijun; Wang, Xiaoqing; Hu, Tuoping; Journal of Solid State Chemistry 261 (2018) 37–42; doi:10.1016/j.jssc.2018.02.007

data_1561140
_publ_section_title
;
 Three novel coordination polymers based on tris(p-carboxyphenyl)phosphane
 oxide: Syntheses, structural characterization and magnetic properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              37
_journal_page_last               42
_journal_paper_doi               10.1016/j.jssc.2018.02.007
_journal_volume                  261
_journal_year                    2018
_chemical_absolute_configuration .
_chemical_formula_moiety         'C78 H68 Co3 N12 O21 P2, 12(H2 O)'
_chemical_formula_sum            'C78 H92 Co3 N12 O33 P2'
_chemical_formula_weight         1964.37
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                93.0440(10)
_cell_angle_beta                 110.6830(10)
_cell_angle_gamma                108.3540(10)
_cell_formula_units_Z            1
_cell_length_a                   13.5630(6)
_cell_length_b                   13.5719(6)
_cell_length_c                   13.6512(6)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.645
_cell_measurement_theta_min      3.022
_cell_volume                     2192.77(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39457
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.029
_diffrn_reflns_theta_max         25.029
_diffrn_reflns_theta_min         3.023
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.7849
_exptl_absorpt_correction_T_min  0.6656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1019
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         15165
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+1.6400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10675
_reflns_number_total             15165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           hu0610b1_0m
_cod_database_code               1561140
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.61(2)
 0.39(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O9W) \\sim Ueq, Uanis(O10W) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Riding coordinates:
 O2W(H2Wa,H2Wb), O1W(H1Wa,H1Wb), O3W(H3Wa,H3Wb), O4W(H4Wa,H4Wb), O5W(H5Wa,
 H5Wb), O6W(H6Wa,H6Wb), O7W(H7Wa,H7Wb), O16W(H16a,H16b), O19W(H19a,H19b),
 O14W(H14a,H14b), O8W(H8Wa,H8Wb), O11W(H11a,H11b), O10W(H10a,H10b), O13W(H13a,
 H13b), O18W(H18a,H18b), O12W(H12a,H12b), O17W(H17a,H17b), O9W(H9Wa,H9Wb),
 O15W(H15a,H15b)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C32(H32), C33(H33), C36(H36),
 C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C46(H46), C47(H47), C49(H49),
  C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
  C69(H69), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78)
;
_shelx_res_checksum              78582
_shelx_hkl_checksum              43316
_olex2_submission_special_instructions 'No special instructions were received'