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_4071379
_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         'C30 H32 Cl Cu P2'
_chemical_formula_sum            'C30 H32 Cl Cu P2'
_chemical_formula_weight         553.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0865(18)
_cell_length_b                   21.048(4)
_cell_length_c                   14.503(3)
_cell_measurement_reflns_used    1373
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.489
_cell_measurement_theta_min      2.465
_cell_volume                     2730.2(10)
_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 8.5
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1357
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30759
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  0.990000
_exptl_absorpt_correction_T_min  0.737882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat stalk'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6252
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+6.8258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                4098
_reflns_number_total             6252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800139v-file002.cif
_cod_data_source_block           sd006asad
_cod_original_cell_volume        2730.1(10)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4071379