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_7705396
_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         'F6 Sb, C32 H46 Cu N2 O4, 0.98(C H2 Cl2)'
_chemical_formula_sum            'C32.98 H47.96 Cl1.96 Cu F6 N2 O4 Sb'
_chemical_formula_weight         905.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                108.75(3)
_cell_angle_beta                 92.22(3)
_cell_angle_gamma                91.99(3)
_cell_formula_units_Z            2
_cell_length_a                   11.027(2)
_cell_length_b                   13.071(3)
_cell_length_c                   14.287(3)
_cell_measurement_reflns_used    39588
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.000
_cell_measurement_theta_min      2.448
_cell_volume                     1946.1(8)
_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
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega 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  0.0643
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.448
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.478624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.2206 before and 0.0721 after correction.
The Ratio of minimum to maximum transmission is 0.4786.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       needle
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.920
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         11332
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0270P)^2^+4.8368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8611
_reflns_number_total             11332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02524k2.cif
_cod_data_source_block           sad_CCDC6
_cod_depositor_comments
'Adding full bibliography for 7705390--7705397.cif.'
_cod_database_code               7705396
_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. Rigid bond restraints
 Sb1, F6B, F3B, F5B, F5A, F3A, F4B, F4A, F1, F2, F6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F4A \\sim F4B \\sim F5A \\sim F5B \\sim F3A \\sim F3B \\sim F6A \\sim F1 \\sim
F2 \\sim F6B \\sim Sb1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Sof(Cl1)=Sof(Cl2)=Sof(C33)=Sof(H33A)=Sof(H33B)=FVAR(1)
 Sof(F6B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=1-FVAR(2)
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C14(H14A,H14B), C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C5(H5), C3(H3), C24(H24), C26(H26)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C19(H19A,H19B,
 H19C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C), C20(H20A,H20B,H20C), C32(H32A,
 H32B,H32C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C),
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              92628
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'