Synthesis of Bis(phosphine) and N-Heterocyclic Carbene Supported α- Diazoalkyl Complexes of Copper(I)
Iluc, Vlad M.; Laskowski, Carl A.; Hillhouse, Gregory L.; Organometallics 28 (2009) 6135–; doi:10.1021/om900566k

data_4070009
_publ_section_title
;
 Synthesis of Bis(phosphine) and N-Heterocyclic Carbene Supported \a-
 Diazoalkyl Complexes of Copper(I)
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6135
_journal_paper_doi               10.1021/om900566k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C52 H61 Cu N4'
_chemical_formula_weight         805.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.028(2)
_cell_length_b                   19.667(2)
_cell_length_c                   22.925(3)
_cell_measurement_temperature    100(2)
_cell_volume                     9029.9(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0934
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45643
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.2904
_exptl_absorpt_correction_T_min  0.2188
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Norton et al.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                5772
_reflns_number_total             7945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900566k_si_001.cif
_cod_data_source_block           (IPr)Cu(CN2dmp)
_cod_original_cell_volume        9029.6(18)
_cod_original_sg_symbol_H-M      pbca
_cod_database_code               4070009