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_7705393
_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         'C42 H50 Cu N2 O2, C2.5 H6'
_chemical_formula_sum            'C44.5 H56 Cu N2 O2'
_chemical_formula_weight         714.45
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.352(3)
_cell_length_b                   22.352(3)
_cell_length_c                   33.005(7)
_cell_measurement_reflns_used    53484
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.468
_cell_volume                     16490(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
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0897
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53484
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.468
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.074012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.2201 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.0740.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       plate
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0732P)^2^+25.7279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5520
_reflns_number_total             9388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02524k2.cif
_cod_data_source_block           sad_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7705390--7705397.cif.'
_cod_original_cell_volume        16489(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C44.50 H56 Cu N2 O2'
_cod_database_code               7705393
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C44B-C45B
 1.5 with sigma of 0.02
 C44A-C45A
 1.5 with sigma of 0.02
 C43-C45A
 2.5 with sigma of 0.02
 C43-C45B
 2.5 with sigma of 0.02
 C44B-C43
 1.5 with sigma of 0.02
 C44A-C43
 1.5 with sigma of 0.02
 C44B-C44B_$1
 2.5 with sigma of 0.02
 C43-C45B
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C43, C44B, C45A, C44A, C45B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C45A \\sim C44B \\sim C43 \\sim C44A \\sim C45B: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Others
 Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44A)=Sof(H44A)=Sof(H44B)=1-FVAR(1)
 Sof(C45A)=Sof(H45A)=Sof(H45B)=0.5*(1-FVAR(2))
 Sof(C45B)=Sof(H45C)=Sof(H45D)=0.5*FVAR(2)
 Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44B)=Sof(H44C)=Sof(H44D)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C45A(H45A,H45B), C44A(H44A,H44B), C45B(H45C,H45D), C44B(H44C,H44D)
6.b Me refined with riding coordinates:
 C43(H43D,H43E,H43F), C43(H43A,H43B,H43C)
6.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C5(H5), C7(H7), C18(H18), C19(H19), C28(H28), C3(H3), C17(H17),
 C27(H27), C20(H20), C24(H24), C33(H33), C26(H26), C25(H25)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C38(H38A,H38B,
 H38C), C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C14(H14A,H14B,H14C), C40(H40A,
 H40B,H40C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              76093
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'