Distorted copper(ii) radicals with sterically hindered salens: electronic structure and aerobic oxidation of alcohols.
Kunert, R.; Philouze, C.; Berthiol, F.; Jarjayes, O.; Storr, T.; Thomas, F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12990–13002; doi:10.1039/d0dt02524k

data_7705397
_publ_section_title
;
 Distorted copper(ii) radicals with sterically hindered salens: electronic
 structure and aerobic oxidation of alcohols.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12990
_journal_page_last               13002
_journal_paper_doi               10.1039/d0dt02524k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C36 H38 Cu N2 O4, C0.16 H0.32 Cl0.32'
_chemical_formula_sum            'C36.16 H38.32 Cl0.32 Cu N2 O4'
_chemical_formula_weight         639.60
_space_group_crystal_system      rhombohedral
_space_group_IT_number           148
_space_group_name_Hall           '-P 3*'
_space_group_name_H-M_alt        'R -3 :R'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2020-07-07 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                115.759(17)
_cell_angle_beta                 115.759(17)
_cell_angle_gamma                115.759(17)
_cell_formula_units_Z            6
_cell_length_a                   21.012(2)
_cell_length_b                   21.012(2)
_cell_length_c                   21.012(2)
_cell_measurement_reflns_used    29196
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.497
_cell_measurement_theta_min      2.841
_cell_volume                     4814(5)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29196
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.841
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.500579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1998 before and 0.0597 after correction.
The Ratio of minimum to maximum transmission is 0.5006.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       needle
_exptl_crystal_F_000             2014
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7300
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0349P)^2^+4.6650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4660
_reflns_number_total             7300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02524k2.cif
_cod_data_source_block           sad3
_cod_depositor_comments
'Adding full bibliography for 7705390--7705397.cif.'
_cod_original_cell_volume        4814(2)
_cod_original_sg_symbol_H-M      'R -3:r'
_cod_database_code               7705397
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-C37
 1.8 with sigma of 0.02
 H37A-C37
 0.95 with sigma of 0.02
 H37B-C37
 0.95 with sigma of 0.02
 H37B-H37A
 1.6 with sigma of 0.02
 Cl1-H37B
 2.65 with sigma of 0.02
3. Rigid bond restraints
 O4A, O4B, C36A, C36B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, O4B, O4A, C36A, C36B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O4B \\sim O4A \\sim C36B \\sim C36A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O4B \\sim O4A \\sim C36A \\sim C36B \\sim C29: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Others
 Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(O4B)=1-FVAR(1)
 Sof(O4A)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C37)=Sof(H37A)=Sof(H37B)=0.33333*FVAR(3)
 Sof(Cl1)=0.66666*FVAR(3)
6.a Riding coordinates:
 C37(H37A,H37B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C25(H25), C28(H28), C7(H7), C14(H14), C24(H24), C30(H30),
 C22(H22), C17(H17), C15(H15), C21(H21), C16(H16), C23(H23)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,
 H34C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C12(H12A,H12B,H12C),
 C36A(H36A,H36B,H36C), C36B(H36D,H36E,H36F)
;
_shelx_res_checksum              82416
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'