First Examples of Metal-Organic Frameworks with Pore-Encapsulated [Co(CO)4]− Anions: Facile Synthesis, Crystal Structures and Stability Studies
Xiao, Caihong; Du, Shaowu; Crystals 14 (2024) 731–; doi:10.3390/cryst14080731

data_1572518
_publ_section_title
;
 First Examples of Metal-Organic Frameworks with Pore-Encapsulated
 [Co(CO)4]&#x2212; Anions: Facile Synthesis, Crystal Structures and
 Stability Studies
;
_journal_issue                   8
_journal_name_full               Crystals
_journal_page_first              731
_journal_paper_doi               10.3390/cryst14080731
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C18 H14 Co0.333 N4, 2(C1.333 Co0.333 O1.333)'
_chemical_formula_sum            'C20.67 H14 Co N4 O2.67'
_chemical_formula_weight         419.95
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.6083(6)
_cell_length_b                   11.6083(6)
_cell_length_c                   13.5342(14)
_cell_measurement_reflns_used    4786
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.52
_cell_volume                     1579.4(2)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Mercury70(2x2 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12140
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.524
_exptl_absorpt_coefficient_mu    0.840
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             643
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.738
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4795
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1171P)^2^+0.3895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                4494
_reflns_number_total             4795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIFs.txt
_cod_data_source_block           compound2
_cod_database_code               1572518
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6127
 0.3873
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3A), C4(H4A), C5(H5A), C6(H6A), C8(H8A), C9(H9A),
 C11(H11A), C12(H12A), C14(H14A), C15(H15A), C17(H17A), C18(H18A)
;
_shelx_res_checksum              60951
_shelx_hkl_checksum              51645
_shelx_fab_checksum              27276
_olex2_submission_special_instructions 'No special instructions were received'