Building a cobaloxime-based metal-organic framework for photocatalytic aerobic oxidation of arylboronic acids to phenols.
Xiao, Yonghong; Zhu, Can-Ming; Liang, Rong-Bin; Huang, Yong-Liang; Hai, Chun-Hua; Chen, Jian-Rui; Li, Mian; Zhong, Jian-Ji; Huang, Xiao-Chun; Chemical communications (Cambridge, England) 59 (2023) 2239–2242; doi:10.1039/d2cc06945h

data_7131193
_publ_section_title
;
 Building a cobaloxime-based metal-organic framework for photocatalytic
 aerobic oxidation of arylboronic acids to phenols.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2239
_journal_page_last               2242
_journal_paper_doi               10.1039/d2cc06945h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         '0.333(C240 H204 Cl6 Co6 N24 O158 Zr24)'
_chemical_formula_sum            'C80 H68 Cl2 Co2 N8 O52.67 Zr8'
_chemical_formula_weight         2902.61
_chemical_name_systematic        Zr-TCPCo
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-11-29
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-11-29 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   35.2672(2)
_cell_length_b                   35.2672(2)
_cell_length_c                   35.2672(2)
_cell_measurement_reflns_used    14705
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.5850
_cell_measurement_theta_min      2.7950
_cell_volume                     43864.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00  19.00   0.50    8.00    --    0.00  77.00-180.00   96
  2  \w     87.00 170.00   0.50   32.00    --   94.20  77.00  90.00  166
  3  \w    127.00 152.00   0.50   32.00    --   94.20  77.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0096278000
_diffrn_orient_matrix_UB_12      -0.0322818000
_diffrn_orient_matrix_UB_13      -0.0277662000
_diffrn_orient_matrix_UB_21      0.0287563000
_diffrn_orient_matrix_UB_22      0.0259727000
_diffrn_orient_matrix_UB_23      -0.0201236000
_diffrn_orient_matrix_UB_31      0.0314003000
_diffrn_orient_matrix_UB_32      -0.0138945000
_diffrn_orient_matrix_UB_33      0.0270577000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            50465
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.552
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light gold'
_exptl_crystal_density_diffrn    0.659
_exptl_crystal_description       sphere
_exptl_crystal_F_000             8600
_exptl_crystal_recrystallization_method Solvothermal
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.180
_refine_diff_density_max         1.368
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         8113
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1577P)^2^+13.5551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2155
_refine_ls_wR_factor_ref         0.2250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6692
_reflns_number_total             8113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06945h2.cif
_cod_data_source_block           Zr-TCPCo
_cod_depositor_comments
'Adding full bibliography for 7131193--7131194.cif.'
_cod_original_cell_volume        43864.5(7)
_cod_database_code               7131193
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zr Cl Co'
_chemical_oxdiff_usercomment     Zr-TCPCo
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.534
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O8-C2 = C2-O1
 1.22 with sigma of 0.02
 O7-C4 = C4-O2
 1.22 with sigma of 0.02
 C3-C4 = C2-C1
 1.52 with sigma of 0.02
 O7-O2
 2.113 with sigma of 0.04
 O8-O1
 2.113 with sigma of 0.04
 Co1B-Cl1B \\sim Co1A-Cl1A
 with sigma of 0.02
 Co1A-O10A \\sim Co1B-O10B
 with sigma of 0.02
 O1-C1 \\sim C1-O8
 with sigma of 0.01
 O7-C3 \\sim C3-O2
 with sigma of 0.01
3. Restrained planarity
 O1, C1, C2, Zr2_$1
 with sigma of 0.1
 O2, C4, C3, Zr1_$1
 with sigma of 0.1
 O2, C4, C3, O7
 with sigma of 0.01
 O1, C1, C2, O8
 with sigma of 0.01
4. Rigid bond restraints
 Co1B, N1B, O9B, O10B, C1A, Cl1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Co1A, N1A, O9A, O10A, C11A, Cl1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C1, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C4, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C1, C2, O8, Zr2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O2, C4, C3, O7, Zr1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 Co1A, Co1B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Co1B \\sim N1B \\sim O9B \\sim O10B \\sim C1A \\sim Cl1B: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
Co1A \\sim N1A \\sim O9A \\sim O10A \\sim C11A \\sim Cl1A: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
O1 \\sim C1 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
O2 \\sim C4 \\sim C3: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
O2 \\sim C4 \\sim C3 \\sim O7 \\sim Zr1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O1 \\sim C1 \\sim C2 \\sim O8 \\sim Zr2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Co1A \\sim Co1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Co1B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(O9B) \\sim Ueq, Uanis(O10B)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(Cl1B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(Co1A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O10A)
\\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O8A) \\sim Ueq, Uanis(O7A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
6. Rigid body (RIGU) restrains
 C11, C10, C7, C8, C6, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8A, C7A, C6, C12, C10A, C9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C4, C3, O7, Zr1
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
 O1, C1, C2, O8, Zr2
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
7. Others
 Fixed Sof: Co1A(0.125) O8A(0.25) O7A(0.25) N1A(0.5) O2(0.5) O9A(0.5) H9A(0.5)
 O10A(0.125) H10A(0.125) H10B(0.125) O1(0.5) C11A(0.5) C11(0.4) H11(0.4)
 C10(0.4) H10(0.4) C7(0.4) H7(0.4) C8(0.4) H8(0.4) C4(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) H1C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C2(0.5) O8B(0.25)
 O7B(0.25) Cl1A(0.0625) Co1B(0.125) N1B(0.5) O9B(0.5) H9B(0.5) O10B(0.125)
 H10C(0.125) H10D(0.125) C1A(0.5) Cl1B(0.0625) C8A(0.6) H8A(0.6) C7A(0.6)
 H7A(0.6) C12(0.6) H12(0.6) C10A(0.6) H10E(0.6) O7(0.5) O8(0.5) Cl2(0.125)
8.a Riding coordinates:
 O10A(H10A,H10B), O10B(H10C,H10D)
8.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C7(H7), C8(H8), C8A(H8A), C7A(H7A), C12(H12), C10A(H10E)
8.c Fitted hexagon refined as free rotating group:
 C8A(C7A,C6,C12,C10A,C9)
8.d Tetrahedral OH refined with riding coordinates:
 O9A(H9A), O9B(H9B)
8.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69507
_shelx_hkl_checksum              41870
_shelx_fab_checksum              83091
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.133
_oxdiff_exptl_absorpt_empirical_full_min 0.921