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_7705394
_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, Sb F6, 0.36(C H2 Cl2)'
_chemical_formula_sum            'C36.36 H38.71 Cl0.71 Cu F6 N2 O4 Sb'
_chemical_formula_weight         892.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.840(5)
_cell_length_b                   25.399(5)
_cell_length_c                   16.261(3)
_cell_measurement_reflns_used    41090
_cell_measurement_temperature    200
_cell_measurement_theta_max      67.994
_cell_measurement_theta_min      3.763
_cell_volume                     9433(3)
_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)'
_computing_structure_solution    'ShelXT-2016 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaCCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41090
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         3.763
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_source_target            Cu
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.959
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.320915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1547 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.3209.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       needle
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.840
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4385
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1280P)^2^+10.6247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3638
_reflns_number_total             4385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02524k2.cif
_cod_data_source_block           sad_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7705390--7705397.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7705394
_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
 F3-F4
 2.6 with sigma of 0.02
 F1-F4
 2.6 with sigma of 0.02
 Sb3-F4
 1.8 with sigma of 0.02
 F2-F4
 3.8 with sigma of 0.02
 F00N-F00Q
 2.6 with sigma of 0.02
 F00N-F00P
 2.6 with sigma of 0.02
 F00R-F00P
 2.6 with sigma of 0.02
 F00N-F00R
 2.6 with sigma of 0.02
 F00P-F00Q
 2.6 with sigma of 0.02
 F3-F4
 2.6 with sigma of 0.02
 F3-F1
 2.6 with sigma of 0.02
 F3-F2
 2.6 with sigma of 0.02
 F1-F4
 2.6 with sigma of 0.02
 F1-F2
 2.6 with sigma of 0.02
 Sb3-F4
 1.8 with sigma of 0.02
 F3-Sb3
 1.8 with sigma of 0.02
 F1-Sb3
 1.8 with sigma of 0.02
 F2-Sb3
 1.8 with sigma of 0.02
 F7-Sb2
 1.8 with sigma of 0.02
 F6-Sb2
 1.8 with sigma of 0.02
 Sb2-F5
 1.8 with sigma of 0.02
 Sb2-F8
 1.8 with sigma of 0.02
 Sb2-F9
 1.8 with sigma of 0.02
 F7-F5
 2.6 with sigma of 0.02
 F7-F6
 2.6 with sigma of 0.02
 F7-F8
 2.6 with sigma of 0.02
 F7-F9
 2.6 with sigma of 0.02
 F8-F5
 2.6 with sigma of 0.02
 F8-F6
 2.6 with sigma of 0.02
 F9-F5
 2.6 with sigma of 0.02
 F9-F6
 2.6 with sigma of 0.02
3. Rigid bond restraints
 Sb3, F1, F3, F4, F2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, F6, Sb2, F5, F9, F8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F6, Sb2, F5, F7, F8, F9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Sb3 \\sim F1 \\sim F3 \\sim F4 \\sim F2: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
F6 \\sim Sb2 \\sim F5 \\sim F7 \\sim F8 \\sim F9: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(F9) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(F5) \\sim Ueq, Uanis(F8) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C5)=Sof(H5A)=Sof(H5B)=0.5*FVAR(2)
 Sof(Cl1)=FVAR(1)
 Fixed Sof: Sb1(0.35) F00N(0.7) F00P(0.7) F00Q(0.35) F00R(0.35) Sb3(0.125)
 F3(0.25) F2(0.125) F1(0.25) F4(0.125) Sb2(0.025) F5(0.025) F6(0.025) F7(0.05)
 F8(0.025) F9(0.025)
6.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C00B(H00B), C00D(H00D), C00F(H00F), C00G(H00G), C00I(H00I),
 C00J(H00J)
6.c Idealised Me refined as rotating group:
 C00K(H00A,H00C,H00E), C00L(H00H,H00K,H00L), C00M(H00M,H00N,H00O), C00O(H00P,
 H00Q,H00R)
;
_shelx_res_checksum              55914
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'