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_7242012
_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
'C34 H32 Co N2 O14 P4 Si, C10 H16 Co N2 O4, 6(H2 O)'
_chemical_formula_sum            'C44 H60 Co2 N4 O24 P4 Si'
_chemical_formula_weight         1298.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-10-06 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                67.608(2)
_cell_angle_beta                 88.443(2)
_cell_angle_gamma                64.186(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8494(14)
_cell_length_b                   14.9534(13)
_cell_length_c                   15.0980(13)
_cell_measurement_reflns_used    6069
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      52.148
_cell_measurement_theta_min      2.958
_cell_volume                     2751.4(4)
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17347
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.074
_diffrn_reflns_theta_min         1.479
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         10789
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0684P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7145
_reflns_number_total             10789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01508c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7241867--7242014.cif.'
_cod_database_code               7242012
_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, All O(H,H) groups
2. Restrained distances
 Co2-H17A \\sim Co2-H17B
 with sigma of 0.02
 Co2-H18A \\sim Co2-H18B
 with sigma of 0.02
 Co2-H16A \\sim Co2-H16B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(O24)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(O10A)=Sof(O11A)=Sof(H11A)=Sof(O12A)=1-FVAR(2)
 Sof(O10)=Sof(H10)=Sof(O11)=Sof(O12)=FVAR(2)
5.a Riding coordinates:
 O3(H3), O6(H6), O10(H10), O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B),
 O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B), O20(H20A,H20B), O19(H19A,H19B),
  O23(H23A,H23B), O21(H21A,H21B), O22(H22A,H22B), O24(H24A,H24B), O24A(H24C,
 H24D), O11A(H11A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C5(H5), C6(H6A), C8(H8A), C9(H9), C11(H11), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C32(H32),
  C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C33(H33), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45)
5.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_shelx_res_checksum              89480
_olex2_submission_special_instructions 'No special instructions were received'