Fabrication of new structures from a 3D cobalt phosphonate network: structural transformation and proton conductivity investigation
Min, Xue; Tian, Hong-rui; Li, Ming; Tian, Di; CrystEngComm 23 (2021) 876–883; doi:10.1039/D0CE01508C

data_7242011
_publ_section_title
;
 Fabrication of new structures from a 3D cobalt phosphonate network:
 structural transformation and proton conductivity investigation
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              876
_journal_page_last               883
_journal_paper_doi               10.1039/D0CE01508C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C44 H40 Co2 N4 O14 P4 Si, O'
_chemical_formula_sum            'C44 H42 Co2 N4 O15 P4 Si'
_chemical_formula_weight         1136.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-10-06 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8502(5)
_cell_length_b                   25.0643(10)
_cell_length_c                   15.0803(6)
_cell_measurement_reflns_used    5508
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.047
_cell_measurement_theta_min      1.597
_cell_volume                     4772.3(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.047
_diffrn_reflns_theta_min         1.597
_exptl_absorpt_coefficient_mu    0.928
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             2328
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9409
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0656P)^2^+3.1096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7155
_reflns_number_total             9409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01508c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7241867--7242014.cif.'
_cod_database_code               7242011
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O13-H13A = O13-H13B
 0.85 with sigma of 0.02
 H13A-H13B
 1.513 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C11(H11A), C2(H2), C12(H12), C20(H20), C14(H14), C17(H17), C22(H22),
  C23(H23), C3(H3A), C6(H6A), C9(H9A), C18(H18), C8(H8), C19(H19), C5(H5),
 C15(H15), C27(H27), C32(H32), C25(H25), C28(H28), C34(H34), C26(H26), C33(H33),
  C42(H42), C44(H44), C38(H38), C37(H37), C36(H36), C43(H43), C41(H41), C35(H35)
4.b Idealised tetrahedral OH refined as rotating group:
 O11(H11), O6(H6), O3(H3), O9(H9)
;
_shelx_res_checksum              36647
_olex2_submission_special_instructions 'No special instructions were received'