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#$Date: 2024-08-05 22:01:52 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/63/7716393.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_7716393
loop_
_publ_author_name
'Hulushe, Siya T.'
'Watkins, Gareth M.'
'Khanye, Setshaba D.'
_publ_section_title
;
 A cobalt(II) coordination polymer-derived catalyst engineered via
 temperature-induced semi-reversible single-crystal-to-single-crystal
 (SCSC) dehydration for efficient liquid-phase epoxidation of olefins.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11326
_journal_page_last               11343
_journal_paper_doi               10.1039/d4dt00739e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C5 H3 Co O5'
_chemical_formula_sum            'C5 H3 Co O5'
_chemical_formula_weight         202.00
_chemical_name_common            'dicobalt(II) pyromellitate dihydrate'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2024-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                113.881(5)
_cell_angle_beta                 99.313(6)
_cell_angle_gamma                93.915(6)
_cell_formula_units_Z            2
_cell_length_a                   3.3576(6)
_cell_length_b                   9.0091(16)
_cell_length_c                   9.5434(15)
_cell_measurement_reflns_used    3171
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      2.386
_cell_volume                     257.61(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.54
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-IV CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11857
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.125
_diffrn_reflns_theta_max         25.369
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.286
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction.
wR2(int) was 0.1117 before and 0.0891 after correction.
The Ratio of minimum to maximum transmission is 0.7525.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.604
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0624
_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/[σ²(Fo²)+(0.0405P)²+2.8013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                695
_reflns_number_total             927
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00739e2.cif
_cod_data_source_block           SOLVE_4M_a
_cod_depositor_comments
'Adding full bibliography for 7716391--7716393.cif.'
_cod_original_cell_volume        257.60(8)
_cod_database_code               7716393
_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.
;
_shelx_estimated_absorpt_t_min   0.489
_shelx_estimated_absorpt_t_max   0.793
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.000000 1.000000 0.500000 0.0358(5) Uani 1 2 d S . P . .
Co2 Co 0.500000 0.500000 0.000000 0.0365(5) Uani 1 2 d S . P . .
O2 O 0.0609(17) 0.5491(7) 0.1533(6) 0.0373(13) Uani 1 1 d . . . . .
O4 O 0.4735(17) 0.0473(7) 0.3865(7) 0.0385(14) Uani 1 1 d . . . . .
O3 O 0.6230(18) 0.1121(7) 0.1991(7) 0.0405(14) Uani 1 1 d . . . . .
O5W O 0.5325(18) 0.7424(7) 0.0270(7) 0.0422(14) Uani 1 1 d . . . . .
H5WA H 0.539842 0.805633 0.122285 0.063 Uiso 1 1 d R U . . .
H5WB H 0.322861 0.751536 -0.030594 0.063 Uiso 1 1 d R U . . .
O1 O -0.0722(17) 0.7663(7) 0.3456(6) 0.0362(13) Uani 1 1 d . . . . .
C4 C 0.530(2) 0.3305(10) 0.4269(9) 0.0330(18) Uani 1 1 d . . . . .
C2 C 0.320(2) 0.5793(10) 0.4111(9) 0.0315(17) Uani 1 1 d . . . . .
C1 C 0.100(2) 0.6419(10) 0.2991(10) 0.0336(18) Uani 1 1 d . . . . .
C3 C 0.359(2) 0.4134(10) 0.3427(9) 0.0340(18) Uani 1 1 d . . . . .
H3 H 0.262691 0.353929 0.232826 0.041 Uiso 1 1 calc R U . . .
C5 C 0.549(2) 0.1528(10) 0.3290(10) 0.0345(18) 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'
Co Co 0.3494 0.9721 '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'
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
O1 Co1 O1 180.0 2_576 . ?
O1 Co1 O4 93.5(2) 2_576 2_666 ?
O1 Co1 O4 86.5(2) . 2_666 ?
O1 Co1 O4 86.5(2) 2_576 1_465 ?
O1 Co1 O4 93.5(2) . 1_465 ?
O4 Co1 O4 180.0 2_666 1_465 ?
O1 Co1 O4 87.1(2) 2_576 2_566 ?
O1 Co1 O4 92.9(2) . 2_566 ?
O4 Co1 O4 104.2(2) 2_666 2_566 ?
O4 Co1 O4 75.8(2) 1_465 2_566 ?
O1 Co1 O4 92.9(2) 2_576 1_565 ?
O1 Co1 O4 87.1(2) . 1_565 ?
O4 Co1 O4 75.8(2) 2_666 1_565 ?
O4 Co1 O4 104.2(2) 1_465 1_565 ?
O4 Co1 O4 180.0 2_566 1_565 ?
O5W Co2 O5W 180.0 2_665 . ?
O5W Co2 O2 92.4(2) 2_665 2_565 ?
O5W Co2 O2 87.6(2) . 2_565 ?
O5W Co2 O2 87.6(2) 2_665 1_655 ?
O5W Co2 O2 92.4(2) . 1_655 ?
O2 Co2 O2 180.0(3) 2_565 1_655 ?
O5W Co2 O2 88.8(2) 2_665 2_665 ?
O5W Co2 O2 91.2(2) . 2_665 ?
O2 Co2 O2 103.6(2) 2_565 2_665 ?
O2 Co2 O2 76.4(2) 1_655 2_665 ?
O5W Co2 O2 91.2(2) 2_665 . ?
O5W Co2 O2 88.8(2) . . ?
O2 Co2 O2 76.4(2) 2_565 . ?
O2 Co2 O2 103.6(2) 1_655 . ?
O2 Co2 O2 180.0 2_665 . ?
C1 O2 Co2 120.2(5) . 1_455 ?
C1 O2 Co2 131.4(5) . . ?
Co2 O2 Co2 103.6(2) 1_455 . ?
C5 O4 Co1 112.9(5) . 1_645 ?
C5 O4 Co1 134.5(5) . 1_545 ?
Co1 O4 Co1 104.2(2) 1_645 1_545 ?
Co2 O5W H5WA 109.5 . . ?
Co2 O5W H5WB 109.2 . . ?
H5WA O5W H5WB 109.4 . . ?
C1 O1 Co1 144.1(5) . . ?
C3 C4 C2 117.8(7) . 2_666 ?
C3 C4 C5 114.5(7) . . ?
C2 C4 C5 127.6(7) 2_666 . ?
C3 C2 C4 118.8(7) . 2_666 ?
C3 C2 C1 114.5(7) . . ?
C4 C2 C1 126.7(7) 2_666 . ?
O1 C1 O2 121.8(7) . . ?
O1 C1 C2 121.9(7) . . ?
O2 C1 C2 115.8(7) . . ?
C4 C3 C2 123.4(7) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
O3 C5 O4 122.5(8) . . ?
O3 C5 C4 119.4(7) . . ?
O4 C5 C4 118.1(7) . . ?
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 O1 1.992(5) 2_576 ?
Co1 O1 1.992(5) . ?
Co1 O4 2.082(5) 2_666 ?
Co1 O4 2.082(5) 1_465 ?
Co1 O4 2.173(6) 2_566 ?
Co1 O4 2.173(6) 1_565 ?
Co2 O5W 2.086(6) 2_665 ?
Co2 O5W 2.086(6) . ?
Co2 O2 2.087(5) 2_565 ?
Co2 O2 2.087(5) 1_655 ?
Co2 O2 2.185(6) 2_665 ?
Co2 O2 2.185(6) . ?
O2 C1 1.279(10) . ?
O4 C5 1.305(10) . ?
O3 C5 1.216(10) . ?
O5W H5WA 0.8507 . ?
O5W H5WB 0.8506 . ?
O1 C1 1.248(9) . ?
C4 C3 1.390(10) . ?
C4 C2 1.407(11) 2_666 ?
C4 C5 1.504(11) . ?
C2 C3 1.393(11) . ?
C2 C1 1.514(10) . ?
C3 H3 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5W H5WA O4 0.85 2.64 3.467(8) 165.6 1_565
O5W H5WA O3 0.85 2.53 3.025(8) 117.7 1_565
O5W H5WA O1 0.85 2.48 3.030(8) 123.3 1_655
O5W H5WB O3 0.85 2.41 2.944(8) 121.7 2_665
