A Three Coordinate Copper(II) Alkynyl Complex in C-C Bond Formation: The Sesquicentennial of the Glaser Coupling.
Bakhoda, Abolghasem; Okoromoba, Otome E.; Greene, Christine; Raghibi Boroujeni, Mahdi; Bertke, Jeffery A.; Warren, Timothy H.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07137

data_4135299
_publ_section_title
;
 A Three Coordinate Copper(II) Alkynyl Complex in C-C Bond Formation: The
 Sesquicentennial of the Glaser Coupling.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07137
_journal_year                    2020
_chemical_formula_moiety         '2(C37 H44 Cl2 Cu N2), C5 H12'
_chemical_formula_sum            'C79 H100 Cl4 Cu2 N4'
_chemical_formula_weight         1374.50
_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
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.545(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.325(2)
_cell_length_b                   10.6380(8)
_cell_length_c                   23.8621(18)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.19
_cell_volume                     7443.7(9)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2018-1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      101(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52205
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.418
_diffrn_reflns_theta_min         2.084
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         13691
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+54.4839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8746
_reflns_number_total             13691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c07137_si_003.cif
_cod_data_source_block           B18411_a
_cod_original_cell_volume        7443.6(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4135299
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.787
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              10669
_shelx_hkl_checksum              47452