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_7131194
_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         'C25 H16 O'
_chemical_formula_sum            'C25 H16 O'
_chemical_formula_weight         332.38
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-27
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2022-11-27 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.8049(2)
_cell_length_b                   10.8049(2)
_cell_length_c                   12.9961(2)
_cell_measurement_reflns_used    6683
_cell_measurement_temperature    298.62(10)
_cell_measurement_theta_max      70.4150
_cell_measurement_theta_min      3.3650
_cell_volume                     1313.97(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.62(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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    -17.00  87.00   0.50    0.50    --    0.00  38.00  60.00  208
  2  \w     39.00  73.00   0.50    0.50    --    0.00  77.00-150.00   68
  3  \w    -23.00  13.00   0.50    0.50    --    0.00  77.00-150.00   72
  4  \w     74.00 175.00   0.50    0.50    --   89.30  45.00-120.00  202
  5  \w     64.00 105.00   0.50    0.50    --   89.30 -30.00  30.00   82
  6  \w     74.00 172.00   0.50    0.50    --   89.30  30.00-150.00  196
  7  \w      9.00 105.00   0.50    0.50    --   89.30 -45.00  60.00  192
  8  \w     76.00 177.00   0.50    0.50    --   89.30  30.00  90.00  202
  9  \w    111.00 179.00   0.50    0.50    --   89.30  15.00  30.00  136
 10  \w     99.00 161.00   0.50    0.50    --   89.30  30.00 120.00  124
 11  \w    115.00 176.00   0.50    0.50    --   89.30  30.00  60.00  122
 12  \w    127.00 153.00   0.50    0.50    --   89.30  30.00 150.00   52
 13  \w     78.00 103.00   0.50    0.50    --   89.30  30.00  60.00   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      0.0529929000
_diffrn_orient_matrix_UB_12      -0.0193194000
_diffrn_orient_matrix_UB_13      0.1056714000
_diffrn_orient_matrix_UB_21      0.0118572000
_diffrn_orient_matrix_UB_22      -0.1266305000
_diffrn_orient_matrix_UB_23      -0.0427287000
_diffrn_orient_matrix_UB_31      0.1553573000
_diffrn_orient_matrix_UB_32      0.1033430000
_diffrn_orient_matrix_UB_33      -0.0327080000
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8564
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.971
_diffrn_reflns_theta_min         4.726
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63934
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       irregular
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1469 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0601
_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^)+(0.1332P)^2^+0.0773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                3153
_reflns_number_total             3271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06945h2.cif
_cod_data_source_block           O19
_cod_depositor_comments
'Adding full bibliography for 7131193--7131194.cif.'
_cod_original_cell_volume        1313.97(5)
_cod_database_code               7131194
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N'
_chemical_oxdiff_usercomment     'zhongjianji zhucanming'
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.800
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
O2 \\sim C10 \\sim C11: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
3. Others
 Fixed Sof: H23(0.5) H10(0.5) O1(0.5) H1(0.5) O2(0.5) H2A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C2(H2), C3(H3), C15(H15), C16(H16), C5(H5), C4(H4), C18(H18),
 C17(H17), C23(H23), C11(H11), C21(H21), C8(H8), C22(H22), C10(H10), C9(H9)
4.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2A)
;
_shelx_res_checksum              23660
_shelx_hkl_checksum              8463
_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 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.705