Selective aerobic oxidation of biomass model compound veratryl alcohol catalyzed by air-stable copper(ii) complexes in water
Jana, Narayan Ch.; Behera, Sourav; Maharana, Suraj Kumar; Behera, Rakesh R.; Bagh, Bidraha; Catalysis Science & Technology 13 (2023) 5422–5434; doi:10.1039/D3CY00671A

data_1569596
_publ_section_title
;
 Selective aerobic oxidation of biomass model compound veratryl alcohol
 catalyzed by air-stable copper(ii) complexes in water
;
_journal_issue                   18
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5422
_journal_page_last               5434
_journal_paper_doi               10.1039/D3CY00671A
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C21 H22 Br2 Cu N2 S'
_chemical_formula_sum            'C21 H22 Br2 Cu N2 S'
_chemical_formula_weight         557.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-11-07 deposited with the CCDC.	2023-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.80220(10)
_cell_length_b                   9.47810(10)
_cell_length_c                   13.72300(10)
_cell_measurement_reflns_used    28218
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1750
_cell_measurement_theta_min      4.7040
_cell_volume                     2177.19(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -42.00  27.00   0.50    0.35    --  -38.50  43.00  57.00  138
  2  \w   -103.00 -34.00   0.50    0.35    --  -38.50 -43.00 -94.00  138
  3  \w     45.00 114.00   0.50    0.35    --   48.56  43.00  57.00  138
  4  \w    -16.00  53.00   0.50    0.35    --   48.56 -43.00 -94.00  138
  5  \w     37.00 106.00   0.50    1.40    --  101.38 -43.00 -94.00  138
  6  \w     97.00 166.00   0.50    1.40    --  101.38  43.00  57.00  138
  7  \w    -44.00  31.00   0.50    0.35    --  -38.50  19.00 -90.00  150
  8  \w   -105.00 -35.00   0.50    0.35    --  -38.50 -37.00 -60.00  140
  9  \w     37.00 112.00   0.50    0.35    --   48.56  57.00 -30.00  150
 10  \w    -18.00  52.00   0.50    0.35    --   48.56 -37.00  60.00  140
 11  \w     28.00 100.00   0.50    0.35    --   48.56-125.00 120.00  144
 12  \w     37.00 106.00   0.50    1.40    --  101.38 -45.00  30.00  138
 13  \w     33.00 105.00   0.50    1.40    --  101.38 -30.00 -60.00  144
 14  \w    104.00 171.00   0.50    1.40    --  101.38 111.00 -30.00  134
 15  \w     33.00 107.00   0.50    1.40    --  101.38 -94.00  60.00  148
 16  \w     88.00 164.00   0.50    1.40    --  101.38  61.00 150.00  152
 17  \w     32.00 109.00   0.50    1.40    --  101.38-111.00-150.00  154
 18  \w     98.00 170.00   0.50    1.40    --  101.38  30.00  90.00  144
 19  \w    103.00 166.00   0.50    1.40    --  101.38  77.00 -90.00  126
 20  \w     32.00 109.00   0.50    1.40    --  101.38-111.00 -60.00  154
 21  \w    104.00 171.00   0.50    1.40    --  101.38 111.00   0.00  134
 22  \w     39.00 115.00   0.50    1.40    --  101.38 -61.00 -60.00  152
 23  \w     33.00 107.00   0.50    1.40    --  101.38 -94.00 -60.00  148
 24  \w     33.00 105.00   0.50    1.40    --  101.38 -30.00 120.00  144
 25  \w     39.00 115.00   0.50    1.40    --  101.38 -61.00 120.00  152
 26  \w     61.00 146.00   0.50    1.40    --  101.38 178.00  90.00  170
 27  \w     32.00 109.00   0.50    1.40    --  101.38-111.00-120.00  154
 28  \w     97.00 166.00   0.50    1.40    --  101.38  45.00 -90.00  138
 29  \w     97.00 166.00   0.50    1.40    --  101.38  45.00 -60.00  138
 30  \w     33.00 107.00   0.50    1.40    --  101.38 -94.00   0.00  148
 31  \w    104.00 171.00   0.50    1.40    --  101.38 111.00  30.00  134
 32  \w     42.00 121.00   0.50    1.40    --  101.38 -77.00  60.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31353
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         5.285
_exptl_absorpt_coefficient_mu    6.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00015(3)
_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   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0332P)^2^+2.4235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3970
_reflns_number_total             3994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00671a2.cif
_cod_data_source_block           nj-cubr
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '100.00 (10)' was
changed to '100(10)' -- precision was estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1569594--1569596.cif.
;
_cod_database_code               1569596
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C1(H1), C3(H3), C4(H4), C17(H17), C21(H21), C18(H18), C19(H19),
 C20(H20), C11(H11), C15(H15), C14(H14), C13(H13), C12(H12)
;
_shelx_res_checksum              12485
_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
;