Electronic Structures and Reactivity Profiles of Aryl Nitrenoid-Bridged Dicopper Complexes.
Carsch, Kurtis M.; Lukens, James T.; DiMucci, Ida M.; Iovan, Diana A.; Zheng, Shao-Liang; Lancaster, Kyle M.; Betley, Theodore A.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b09616

data_4134026
_publ_section_title
;
 Electronic Structures and Reactivity Profiles of Aryl Nitrenoid-Bridged
 Dicopper Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09616
_journal_year                    2020
_chemical_formula_sum            'C96.88 H99.25 Cu2 N4 O P2'
_chemical_formula_weight         1524.57
_chemical_name_systematic        (tBudmx)Cu2(PPh3)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 117.092(7)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   57.196(11)
_cell_length_b                   25.306(4)
_cell_length_c                   26.078(3)
_cell_measurement_reflns_used    9125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.38
_cell_volume                     33604(9)
_computing_cell_refinement       'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX3 v2016.1.0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT 8.35A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            281841
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.225
_diffrn_reflns_theta_max         25.225
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             12872
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.136
_refine_diff_density_max         1.418
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.095
_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     1990
_refine_ls_number_reflns         30048
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0648P)^2^+266.8993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19269
_reflns_number_total             30048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09616_si_002.cif
_cod_data_source_block           13
_cod_original_cell_volume        33604(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4134026
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              89978
_shelx_hkl_checksum              40053