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_1569594
_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 H20 Br2 Cu N2 S'
_chemical_formula_sum            'C21 H20 Br2 Cu N2 S'
_chemical_formula_weight         555.81
_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             2022-01-17
_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                90.000(3)
_cell_angle_beta                 90.946(3)
_cell_angle_gamma                90.000(3)
_cell_formula_units_Z            4
_cell_length_a                   10.9864(4)
_cell_length_b                   12.8237(4)
_cell_length_c                   15.4669(5)
_cell_measurement_reflns_used    8818
_cell_measurement_temperature    298(90)
_cell_measurement_theta_max      29.5520
_cell_measurement_theta_min      3.5620
_cell_volume                     2178.78(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      298(90)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.816
_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     -1.00  24.00   0.50   14.68    --    3.51-101.00 117.00   50
  2  \w    -13.00  33.00   0.50   14.68    --   -4.14-101.00 117.00   92
  3  \w     11.00  37.00   0.50   14.68    --    3.51 -99.00   0.00   52
  4  \w     -9.00  21.00   0.50   14.68    --   -4.14  77.00  90.00   60
  5  \w     18.00  59.00   0.50   14.68    --   -4.14  57.00-120.00   82
  6  \w    -27.00  12.00   0.50   14.68    --   -4.14  77.00  60.00   78
  7  \w    -39.00  -2.00   0.50   14.68    --   -4.14 -77.00 -30.00   74
  8  \w    -16.00  15.00   0.50   14.68    --   -4.14  57.00-120.00   62
  9  \w    -27.00  10.00   0.50   14.68    --   -4.14  77.00 -30.00   74
 10  \w    -27.00  20.00   0.50   14.68    --   -4.14  77.00 -60.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0190084000
_diffrn_orient_matrix_UB_12      0.0121115000
_diffrn_orient_matrix_UB_13      -0.0424391000
_diffrn_orient_matrix_UB_21      0.0593294000
_diffrn_orient_matrix_UB_22      -0.0183647000
_diffrn_orient_matrix_UB_23      0.0104417000
_diffrn_orient_matrix_UB_31      -0.0169719000
_diffrn_orient_matrix_UB_32      -0.0507488000
_diffrn_orient_matrix_UB_33      -0.0139114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23815
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.462
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+2.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4158
_reflns_number_total             5406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00671a2.cif
_cod_data_source_block           nj-99
_cod_depositor_comments
'Adding full bibliography for 1569594--1569596.cif.'
_cod_database_code               1569594
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C84 H80 Br8 Cu4 N8 S4 '
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.449
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C1(H1), C11(H11), C2(H2), C15(H15), C17(H17),
 C14(H14), C21(H21), C13(H13), C12(H12), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              68142
_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 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.791