Copper(I) Diphosphine Catalysts for C−N Bond Formation: Synthesis, Structure, and Ligand Effects
Daly, Stephen; Haddow, Mairi F.; Orpen, A. Guy; Rolls, Giles T. A.; Wass, Duncan F.; Wingad, Richard L.; Organometallics 27 (2008) 3196–; doi:10.1021/om800139v

data_4071377
_publ_section_title
;
 Copper(I) Diphosphine Catalysts for C&#x2212;N Bond Formation: Synthesis,
 Structure, and Ligand Effects
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3196
_journal_paper_doi               10.1021/om800139v
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C75 H66 Cl3 Cu3 P6, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C79 H74 Cl7 Cu3 P6'
_chemical_formula_weight         1647.97
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.24(3)
_cell_angle_beta                 90.30(3)
_cell_angle_gamma                90.96(3)
_cell_formula_units_Z            2
_cell_length_a                   13.596(3)
_cell_length_b                   14.178(3)
_cell_length_c                   19.478(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.069
_cell_measurement_theta_min      3.118
_cell_volume                     3754.0(14)
_computing_cell_refinement       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_collection       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT V6.0 (Bruker, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V6.1 (Bruker AXS, 2000)'
_computing_publication_material  'Bruker SHELXTL V6.1 (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29546
_diffrn_reflns_theta_full        70.07
_diffrn_reflns_theta_max         70.07
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.822
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         12807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0828P)^2^+2.8464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                10401
_reflns_number_total             12807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800139v-file002.cif
_cod_data_source_block           sd004sad
_cod_original_cell_volume        3754.2(13)
_cod_database_code               4071377