Aerobic intramolecular carbon-hydrogen bond oxidation promoted by Cu(I) complexes.
Álvarez, María; Molina, Francisco; Fructos, Manuel R.; Urbano, Juan; Álvarez, Eleuterio; Sodupe, Mariona; Lledós, Agustí; Pérez, Pedro J; Dalton transactions (Cambridge, England : 2003) 49 (2020) 14647–14655; doi:10.1039/d0dt03198d

data_7705464
_publ_section_title
;
 Aerobic intramolecular carbon-hydrogen bond oxidation promoted by Cu(I)
 complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14647
_journal_page_last               14655
_journal_paper_doi               10.1039/d0dt03198d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H45 B Cu N7'
_chemical_formula_sum            'C43 H45 B Cu N7'
_chemical_formula_weight         734.21
_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
_audit_creation_date             2017-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2020-05-14 deposited with the CCDC.	2020-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4925(7)
_cell_length_b                   11.5549(4)
_cell_length_c                   16.8158(6)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.38
_cell_volume                     3787.4(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker Apex3, 2017'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type
'Bruker CHi Fixed D8 Quest Photon 100 Detector Apex3'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            147356
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.256
_diffrn_reflns_theta_min         2.139
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0707 before and 0.0583 after correction. 
The Ratio of minimum to maximum transmission is 0.9168. 
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method
'Recrystallised from a mixture of dichloromethane-hexane by slow evaporation'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         14508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11800
_reflns_number_total             14508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03198d2.cif
_cod_data_source_block           Complex_1a
_cod_depositor_comments
'Adding full bibliography for 7705460--7705465.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7705464
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C15(H15),
 C20(H20), C21(H21), C25(H25), C27(H27), C32(H32), C33(H33), C37(H37), C39(H39)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a 200 micro/m MITIGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'