#------------------------------------------------------------------------------
#$Date: 2024-08-05 22:01:52 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/63/7716392.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_7716392
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 H Co O4'
_chemical_formula_sum            'C5 H Co O4'
_chemical_formula_weight         183.99
_chemical_name_common            'dicobalt(II) pyromellitate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 115.606(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1151(7)
_cell_length_b                   17.4400(18)
_cell_length_c                   4.5477(4)
_cell_measurement_reflns_used    2801
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.34
_cell_volume                     437.37(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 5.26
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2281
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.110
_diffrn_reflns_theta_max         25.110
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    3.839
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0340
_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)+7.1430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                368
_reflns_number_total             397
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00739e2.cif
_cod_data_source_block           SOLVE_1U_a
_cod_depositor_comments
'Adding full bibliography for 7716391--7716393.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7716392
_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   0.540
_shelx_estimated_absorpt_t_max   0.717
_shelx_res_file
;
TITL D:\SOLVE_1U_a.res in C2/m
    SOLVE_1U_a.res
    created by SHELXL-2016/6 at 23:22:17 on 05-Jun-2023
CELL 0.71073 6.1151 17.4400 4.5477 90.000 115.606 90.000
ZERR 4.0000 0.0007 0.0018 0.0004 0.000 0.004 0.000
LATT 7
SYMM -X, Y, -Z
SFAC C H O CO
UNIT 20 4 16 4
BOND $H
ACTA 50.25
FMAP 2 1 53
PLAN 20 0 0
HTAB 2.0
LIST 4 1
SIZE 0.183 0.174 0.093
TEMP -123.15
L.S. 10
WGHT    0.000000    7.143000
EXTI    0.009359
FVAR       0.89191
CO1   4    0.500000    0.710172    1.000000    10.50000    0.01332    0.00937 =
         0.01251    0.00000    0.00428    0.00000
O2    3    0.240275    0.700152    0.212833    11.00000    0.01237    0.01009 =
         0.01155    0.00056    0.00556    0.00068
O1    3    0.293343    0.634052    0.656437    11.00000    0.01608    0.01195 =
         0.00923   -0.00121    0.00641   -0.00157
C2    1    0.089644    0.569921    0.159213    11.00000    0.02038    0.00833 =
         0.01336    0.00032    0.01104    0.00076
C3    1    0.174299    0.500000    0.312489    10.50000    0.01421    0.00985 =
         0.01151    0.00000    0.00453    0.00000
AFIX  43
H3    2    0.295271    0.500001    0.531517    10.50000   -1.20000
AFIX   0
C1    1    0.213277    0.639903    0.354980    11.00000    0.00709    0.01351 =
         0.01444    0.00084    0.00538    0.00558
HKLF 4




REM  D:\SOLVE_1U_a.res in C2/m
REM R1 =  0.0340 for     368 Fo > 4sig(Fo)  and  0.0401 for all     397 data
REM     49 parameters refined using      0 restraints

END

WGHT      0.0000      7.1426

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  0.859,  deepest hole -0.616,  1-sigma level  0.147
Q1    1   0.0000  0.6386  0.0000  10.50000  0.05    0.86
Q2    1   0.3960  0.5000  0.8481  10.50000  0.05    0.57
Q3    1   0.2370  0.6170  0.7814  11.00000  0.05    0.55
Q4    1   0.3062  0.4366  0.6388  11.00000  0.05    0.49
Q5    1   0.0000  0.5631  0.0000  10.50000  0.05    0.43
Q6    1   0.3056  0.6955  0.1117  11.00000  0.05    0.40
Q7    1   0.0682  0.5969  0.2198  11.00000  0.05    0.39
Q8    1   0.1558  0.6892  0.0446  11.00000  0.05    0.39
Q9    1   0.1029  0.6430  0.8360  11.00000  0.05    0.39
Q10   1   0.1288  0.6586  0.6133  11.00000  0.05    0.38
Q11   1   0.2143  0.7337  0.2158  11.00000  0.05    0.38
Q12   1   0.5000  0.5000  0.5000  10.25000  0.05    0.38
Q13   1   0.3763  0.6582  0.7902  11.00000  0.05    0.37
Q14   1   0.2367  0.6894  0.8466  11.00000  0.05    0.36
Q15   1   0.1165  0.6002  0.5062  11.00000  0.05    0.35
Q16   1   0.3275  0.5736  0.1658  11.00000  0.05    0.34
Q17   1   0.2029  0.5000  0.6411  10.50000  0.05    0.33
Q18   1   0.5863  0.6331  0.9525  11.00000  0.05    0.33
Q19   1   0.2775  0.5393  0.8182  11.00000  0.05    0.32
Q20   1   0.2047  0.6716  0.2206  11.00000  0.05    0.32
;
_shelx_res_checksum              38262
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.500000 0.71017(5) 1.000000 0.0122(5) Uani 1 2 d S T P . .
O2 O 0.2403(5) 0.70015(17) 0.2128(7) 0.0112(7) Uani 1 1 d . . . . .
O1 O 0.2933(6) 0.63405(17) 0.6564(7) 0.0121(7) Uani 1 1 d . . . . .
C2 C 0.0896(9) 0.5699(2) 0.1592(11) 0.0127(10) Uani 1 1 d . . . . .
C3 C 0.1743(12) 0.500000 0.3125(16) 0.0122(13) Uani 1 2 d S T P . .
H3 H 0.295271 0.500001 0.531517 0.015 Uiso 1 2 calc R U P . .
C1 C 0.2133(8) 0.6399(2) 0.3550(11) 0.0114(10) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0133(6) 0.0094(6) 0.0125(6) 0.000 0.0043(4) 0.000
O2 0.0124(16) 0.0101(16) 0.0116(16) 0.0006(12) 0.0056(13) 0.0007(12)
O1 0.0161(17) 0.0120(15) 0.0092(16) -0.0012(12) 0.0064(14) -0.0016(12)
C2 0.020(2) 0.008(2) 0.013(2) 0.0003(17) 0.011(2) 0.0008(18)
C3 0.014(3) 0.010(3) 0.012(3) 0.000 0.005(3) 0.000
C1 0.007(2) 0.014(2) 0.014(2) 0.0008(17) 0.0054(19) 0.0056(17)
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'
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
O1 Co1 O1 97.99(18) . 2_657 ?
O1 Co1 O2 159.07(12) . 8_566 ?
O1 Co1 O2 93.11(12) 2_657 8_566 ?
O1 Co1 O2 93.11(12) . 7_566 ?
O1 Co1 O2 159.07(12) 2_657 7_566 ?
O2 Co1 O2 82.28(17) 8_566 7_566 ?
O1 Co1 O2 87.64(12) . 1_556 ?
O1 Co1 O2 86.37(12) 2_657 1_556 ?
O2 Co1 O2 110.82(12) 8_566 1_556 ?
O2 Co1 O2 76.38(13) 7_566 1_556 ?
O1 Co1 O2 86.37(12) . 2_656 ?
O1 Co1 O2 87.64(12) 2_657 2_656 ?
O2 Co1 O2 76.38(13) 8_566 2_656 ?
O2 Co1 O2 110.82(12) 7_566 2_656 ?
O2 Co1 O2 170.87(16) 1_556 2_656 ?
C1 O2 Co1 129.3(3) . 7_566 ?
C1 O2 Co1 124.3(3) . 1_554 ?
Co1 O2 Co1 103.62(12) 7_566 1_554 ?
C1 O1 Co1 127.9(3) . . ?
C2 C2 C3 118.6(3) 2 . ?
C2 C2 C1 125.8(2) 2 . ?
C3 C2 C1 115.6(4) . . ?
C2 C3 C2 122.8(6) . 6_565 ?
C2 C3 H3 118.6 . . ?
C2 C3 H3 118.6 6_565 . ?
O1 C1 O2 123.2(4) . . ?
O1 C1 C2 116.2(4) . . ?
O2 C1 C2 120.5(4) . . ?
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 2.023(3) . ?
Co1 O1 2.023(3) 2_657 ?
Co1 O2 2.077(3) 8_566 ?
Co1 O2 2.077(3) 7_566 ?
Co1 O2 2.195(3) 1_556 ?
Co1 O2 2.195(3) 2_656 ?
O2 C1 1.281(5) . ?
O1 C1 1.245(5) . ?
C2 C2 1.388(10) 2 ?
C2 C3 1.389(5) . ?
C2 C1 1.507(6) . ?
C3 H3 0.9500 . ?
