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_1572519
_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         'C10 H9 Co0.25 N2, C2 Co0.5 O2'
_chemical_formula_sum            'C12 H9 Co0.75 N2 O2'
_chemical_formula_weight         257.41
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-10
_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                90
_cell_formula_units_Z            8
_cell_length_a                   12.2559(6)
_cell_length_b                   12.2559(6)
_cell_length_c                   15.4132(16)
_cell_measurement_reflns_used    5331
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.12
_cell_volume                     2315.2(3)
_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  'S'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16984
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    1.125
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       prism
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0854P)^2^+0.7148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2475
_reflns_number_total             2654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIFs.txt
_cod_data_source_block           compound3
_cod_database_code               1572519
_shelx_shelxl_version_number     2016/6
_refine_ls_r_factor_ref          0.0466
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50728
 0.49272
2.a Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C5(H5A), C6(H6A), C8(H8A), C9(H9A)
;
_shelx_res_checksum              10352
_shelx_hkl_checksum              20180
_olex2_submission_special_instructions 'No special instructions were received'