#------------------------------------------------------------------------------
#$Date: 2024-09-06 11:51:15 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294649 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/25/1572518.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1572518
loop_
_publ_author_name
'Xiao, Caihong'
'Du, Shaowu'
_publ_section_title
;
 First Examples of Metal-Organic Frameworks with Pore-Encapsulated
 [Co(CO)4]− 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/[σ²(Fo²)+(0.1171P)²+0.3895P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            CIFs.txt
_cod_data_source_block           compound2
_cod_database_code               1572518
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.666667 0.333333 0.55615(5) 0.0251(2) Uani 1 3 d S T P . .
Co2 Co 1.000000 1.000000 0.62769(17) 0.0721(5) Uani 1 3 d S T P . .
Co3 Co 0.666667 0.333333 1.12324(19) 0.0963(8) Uani 1 3 d S T P . .
N1 N 0.7572(4) 0.5097(4) 0.4645(3) 0.0324(9) Uani 1 1 d . . . . .
N2 N 0.7786(5) 0.6556(5) 0.3524(3) 0.0414(10) Uani 1 1 d . . . . .
N3 N 0.5740(4) 0.1572(4) 0.6487(3) 0.0319(9) Uani 1 1 d . . . . .
N4 N 0.5431(5) 0.0192(5) 0.7719(4) 0.0460(11) Uani 1 1 d . . . . .
O1 O 1.1237(9) 1.2713(9) 0.5528(10) 0.141(4) Uani 1 1 d . . . . .
O2 O 1.000000 1.000000 0.8405(12) 0.128(6) Uani 1 3 d S T P . .
O3 O 0.666667 0.333333 0.9102(13) 0.194(12) Uani 1 3 d S T P . .
O4 O 0.5954(11) 0.0749(9) 1.2088(7) 0.119(3) Uani 1 1 d . . . . .
C1 C 0.6957(6) 0.5367(5) 0.3948(4) 0.0370(11) Uani 1 1 d . . . . .
H1A H 0.607231 0.481645 0.376914 0.044 Uiso 1 1 calc R U . . .
C2 C 0.8836(6) 0.6155(6) 0.4675(4) 0.0464(13) Uani 1 1 d . . . . .
H2A H 0.949012 0.625308 0.511938 0.056 Uiso 1 1 calc R U . . .
C3 C 0.8996(7) 0.7045(7) 0.3958(6) 0.0573(16) Uani 1 1 d . . . . .
H3A H 0.977335 0.782665 0.379863 0.069 Uiso 1 1 calc R U . . .
C4 C 0.6284(6) 0.1297(6) 0.7244(4) 0.0413(12) Uani 1 1 d . . . . .
H4A H 0.717172 0.182279 0.742559 0.050 Uiso 1 1 calc R U . . .
C5 C 0.4430(6) 0.0595(7) 0.6513(5) 0.0540(16) Uani 1 1 d . . . . .
H5A H 0.377581 0.053713 0.608522 0.065 Uiso 1 1 calc R U . . .
C6 C 0.4225(7) -0.0275(8) 0.7253(6) 0.072(2) Uani 1 1 d . . . . .
H6A H 0.342888 -0.103503 0.741327 0.087 Uiso 1 1 calc R U . . .
C7 C 0.5717(7) -0.0357(6) 0.8553(5) 0.0487(14) Uani 1 1 d . . . . .
C8 C 0.4896(9) -0.0787(11) 0.9352(7) 0.084(3) Uani 1 1 d . . . . .
H8A H 0.411029 -0.075715 0.934646 0.101 Uiso 1 1 calc R U . . .
C9 C 0.5231(9) -0.1272(11) 1.0176(6) 0.082(3) Uani 1 1 d . . . . .
H9A H 0.466525 -0.155598 1.071965 0.098 Uiso 1 1 calc R U . . .
C10 C 0.6387(7) -0.1341(6) 1.0208(4) 0.0524(14) Uani 1 1 d . . . . .
C11 C 0.7159(11) -0.0954(14) 0.9376(7) 0.094(3) Uani 1 1 d . . . . .
H11A H 0.792459 -0.102143 0.935960 0.113 Uiso 1 1 calc R U . . .
C12 C 0.6833(12) -0.0470(14) 0.8566(7) 0.102(4) Uani 1 1 d . . . . .
H12A H 0.738289 -0.021266 0.801329 0.123 Uiso 1 1 calc R U . . .
C13 C 0.7442(6) 0.7132(5) 0.2702(4) 0.0440(12) Uani 1 1 d . . . . .
C14 C 0.6361(9) 0.7256(9) 0.2758(5) 0.0651(19) Uani 1 1 d . . . . .
H14A H 0.585431 0.701515 0.333300 0.078 Uiso 1 1 calc R U . . .
C15 C 0.5989(9) 0.7753(10) 0.1939(5) 0.070(2) Uani 1 1 d . . . . .
H15A H 0.522287 0.781838 0.197005 0.084 Uiso 1 1 calc R U . . .
C16 C 0.6755(7) 0.8142(6) 0.1095(4) 0.0483(14) Uani 1 1 d . . . . .
C17 C 0.7873(9) 0.8023(11) 0.1073(6) 0.086(3) Uani 1 1 d . . . . .
H17A H 0.839481 0.826570 0.050558 0.103 Uiso 1 1 calc R U . . .
C18 C 0.8234(9) 0.7543(11) 0.1889(7) 0.086(3) Uani 1 1 d . . . . .
H18A H 0.901532 0.750437 0.187787 0.103 Uiso 1 1 calc R U . . .
C19 C 1.0761(10) 1.1637(10) 0.5848(10) 0.093(3) Uani 1 1 d . . . . .
C20 C 1.000000 1.000000 0.7531(19) 0.096(5) Uani 1 3 d S T P . .
C21 C 0.666667 0.333333 0.9934(8) 0.063(3) Uani 1 3 d S T P . .
C22 C 0.6235(12) 0.1765(13) 1.1735(8) 0.094(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N1 90.39(16) . 3_665 ?
N1 Co1 N1 90.39(16) . 2_655 ?
N1 Co1 N1 90.39(16) 3_665 2_655 ?
N1 Co1 N3 90.30(16) 3_665 . ?
N1 Co1 N3 179.3(2) 2_655 2_655 ?
N1 Co1 N3 89.33(16) . 3_665 ?
N1 Co1 N3 90.30(16) . 2_655 ?
N1 Co1 N3 179.3(2) . . ?
N1 Co1 N3 89.33(16) 3_665 2_655 ?
N1 Co1 N3 179.3(2) 3_665 3_665 ?
N1 Co1 N3 89.33(16) 2_655 . ?
N1 Co1 N3 90.30(16) 2_655 3_665 ?
N3 Co1 N3 89.99(16) 2_655 3_665 ?
N3 Co1 N3 89.99(16) 2_655 . ?
N3 Co1 N3 89.99(16) . 3_665 ?
C19 Co2 C19 109.5(4) . 2_765 ?
C19 Co2 C19 109.5(4) . 3_675 ?
C19 Co2 C19 109.5(4) 2_765 3_675 ?
C20 Co2 C19 109.4(4) . . ?
C20 Co2 C19 109.4(4) . 2_765 ?
C20 Co2 C19 109.4(4) . 3_675 ?
C21 Co3 C22 112.7(4) . . ?
C21 Co3 C22 112.7(4) . 2_655 ?
C21 Co3 C22 112.7(4) . 3_665 ?
C22 Co3 C22 106.1(4) . 3_665 ?
C22 Co3 C22 106.1(4) 2_655 3_665 ?
C22 Co3 C22 106.1(4) . 2_655 ?
C1 N1 Co1 125.0(4) . . ?
C1 N1 C2 106.0(5) . . ?
C2 N1 Co1 129.0(4) . . ?
C1 N2 C3 107.6(5) . . ?
C1 N2 C13 125.1(5) . . ?
C3 N2 C13 127.2(5) . . ?
C4 N3 Co1 127.0(4) . . ?
C4 N3 C5 104.3(5) . . ?
C5 N3 Co1 128.1(4) . . ?
C4 N4 C6 106.2(5) . . ?
C4 N4 C7 126.2(5) . . ?
C6 N4 C7 127.6(5) . . ?
N1 C1 N2 110.7(5) . . ?
N1 C1 H1A 124.7 . . ?
N2 C1 H1A 124.7 . . ?
N1 C2 H2A 125.1 . . ?
N1 C2 C3 109.9(5) . . ?
C3 C2 H2A 125.1 . . ?
N2 C3 C2 105.7(5) . . ?
N2 C3 H3A 127.1 . . ?
C2 C3 H3A 127.1 . . ?
N3 C4 N4 113.0(5) . . ?
N3 C4 H4A 123.5 . . ?
N4 C4 H4A 123.5 . . ?
N3 C5 H5A 125.0 . . ?
C6 C5 N3 110.1(5) . . ?
C6 C5 H5A 125.0 . . ?
N4 C6 H6A 126.9 . . ?
C5 C6 N4 106.3(5) . . ?
C5 C6 H6A 126.9 . . ?
C8 C7 N4 121.4(6) . . ?
C8 C7 C12 118.6(6) . . ?
C12 C7 N4 120.1(6) . . ?
C7 C8 H8A 120.0 . . ?
C7 C8 C9 120.0(7) . . ?
C9 C8 H8A 120.0 . . ?
C8 C9 H9A 119.2 . . ?
C10 C9 C8 121.6(7) . . ?
C10 C9 H9A 119.2 . . ?
C9 C10 C11 116.7(6) . . ?
C9 C10 C16 121.8(6) . 1_546 ?
C11 C10 C16 121.4(7) . 1_546 ?
C10 C11 H11A 119.2 . . ?
C12 C11 C10 121.6(8) . . ?
C12 C11 H11A 119.2 . . ?
C7 C12 C11 121.4(8) . . ?
C7 C12 H12A 119.3 . . ?
C11 C12 H12A 119.3 . . ?
C14 C13 N2 119.7(5) . . ?
C14 C13 C18 121.1(6) . . ?
C18 C13 N2 119.1(6) . . ?
C13 C14 H14A 120.2 . . ?
C13 C14 C15 119.7(6) . . ?
C15 C14 H14A 120.2 . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 C14 120.3(7) . . ?
C16 C15 H15A 119.8 . . ?
C15 C16 C10 122.0(6) . 1_564 ?
C17 C16 C10 119.7(6) . 1_564 ?
C17 C16 C15 118.3(6) . . ?
C16 C17 H17A 119.6 . . ?
C16 C17 C18 120.8(7) . . ?
C18 C17 H17A 119.6 . . ?
C13 C18 C17 119.7(7) . . ?
C13 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 . . ?
O1 C19 Co2 177.3(14) . . ?
O2 C20 Co2 180.0 . . ?
O3 C21 Co3 180.0 . . ?
O4 C22 Co3 178.3(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N1 2.164(4) . ?
Co1 N1 2.164(4) 3_665 ?
Co1 N1 2.164(4) 2_655 ?
Co1 N3 2.170(4) 3_665 ?
Co1 N3 2.170(4) . ?
Co1 N3 2.170(4) 2_655 ?
Co2 C19 1.746(11) 3_675 ?
Co2 C19 1.746(11) 2_765 ?
Co2 C19 1.746(11) . ?
Co2 C20 1.70(3) . ?
Co3 C21 1.757(11) . ?
Co3 C22 1.765(13) 2_655 ?
Co3 C22 1.765(13) . ?
Co3 C22 1.765(13) 3_665 ?
N1 C1 1.313(7) . ?
N1 C2 1.364(8) . ?
N2 C1 1.354(7) . ?
N2 C3 1.357(8) . ?
N2 C13 1.454(7) . ?
N3 C4 1.324(7) . ?
N3 C5 1.369(8) . ?
N4 C4 1.330(7) . ?
N4 C6 1.376(9) . ?
N4 C7 1.415(7) . ?
O1 C19 1.168(13) . ?
O2 C20 1.18(3) . ?
O3 C21 1.13(2) . ?
O4 C22 1.158(14) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C3 1.361(9) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9300 . ?
C5 C6 1.356(9) . ?
C6 H6A 0.9300 . ?
C7 C8 1.361(10) . ?
C7 C12 1.366(12) . ?
C8 H8A 0.9300 . ?
C8 C9 1.389(10) . ?
C9 H9A 0.9300 . ?
C9 C10 1.385(11) . ?
C10 C11 1.368(10) . ?
C10 C16 1.496(6) 1_546 ?
C11 H11A 0.9300 . ?
C11 C12 1.369(10) . ?
C12 H12A 0.9300 . ?
C13 C14 1.334(10) . ?
C13 C18 1.358(10) . ?
C14 H14A 0.9300 . ?
C14 C15 1.413(9) . ?
C15 H15A 0.9300 . ?
C15 C16 1.377(10) . ?
C16 C17 1.372(11) . ?
C17 H17A 0.9300 . ?
C17 C18 1.394(10) . ?
C18 H18A 0.9300 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6127
2 0.3873
