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_1561141
_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_formula_moiety         'C33 H23 Co N4 O7 P, H2 O'
_chemical_formula_sum            'C33 H25 Co N4 O8 P'
_chemical_formula_weight         695.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 98.2750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5121(4)
_cell_length_b                   13.7050(5)
_cell_length_c                   24.3437(9)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.09
_cell_volume                     3140.5(2)
_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      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            63360
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         2.949
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+2.0822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6228
_reflns_number_total             7245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           p
_cod_database_code               1561141
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C27A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C25, C28, C26, C30, C27, C29, C30A, C29A, C26A, C27A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C30A)=Sof(H30A)=Sof(C29A)=Sof(H29A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=1-FVAR(1)
 Sof(C26)=Sof(H26)=Sof(C30)=Sof(H30)=Sof(C27)=Sof(H27)=Sof(C29)=Sof(H29)=FVAR(1)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C17(H17), C32(H32), C16(H16), C20(H20), C9(H9), C4(H4),
 C22(H22), C6(H6), C10(H10), C3(H3), C7(H7), C19(H19), C23(H23), C24(H24),
 C13(H13), C12(H12), C26(H26), C30(H30), C27(H27), C29(H29), C30A(H30A),
 C29A(H29A), C26A(H26A), C27A(H27A)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              32071
_shelx_hkl_checksum              26111
_olex2_submission_special_instructions 'No special instructions were received'