Chan–Evans–Lam Couplings with Copper Iminoarylsulfonate Complexes: Scope and Mechanism
Hardouin Duparc, Valérie; Bano, Guillaume L.; Schaper, Frank; ACS Catalysis 8 (2018) 7308–; doi:10.1021/acscatal.8b01881

data_4515563
_publ_section_title
;
 Chan--Evans--Lam Couplings with Copper Iminoarylsulfonate Complexes:
 Scope and Mechanism
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              7308
_journal_paper_doi               10.1021/acscatal.8b01881
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C26 H22 Cu N4 O6 S2, H2 O'
_chemical_formula_sum            'C26 H24 Cu N4 O7 S2'
_chemical_formula_weight         632.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   dual
_audit_creation_date             2017-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7588(4)
_cell_length_b                   13.9390(3)
_cell_length_c                   20.7682(4)
_cell_measurement_reflns_used    9290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.70
_cell_measurement_theta_min      3.70
_cell_volume                     5140.96(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66841
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.693
_diffrn_reflns_theta_min         3.703
_diffrn_source                   'Metal Jet'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.891
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1414 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.6352.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       blcok
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0490P)^2^+4.3793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5566
_reflns_number_total             5895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b01881_si_002.cif
_cod_data_source_block           comp2
_cod_database_code               4515563
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.452
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Free rotating group:
 O7(H7A)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C19(H19), C21(H21), C22(H22), C24(H24)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              1807
_shelx_hkl_checksum              45605
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'