Synthesis and Structure of Intermediates in Copper-Catalyzed Alkylation of Diphenylphosphine
Matthew F. Cain; Russell P. Hughes; David S. Glueck; James A. Golen; Curtis E. Moore; Arnold L. Rheingold; Inorganic Chemistry 49 (2010) 7650–7662; doi:10.1021/ic100816u

data_4316385
_publ_section_title
;
 Synthesis and Structure of Intermediates in Copper-Catalyzed Alkylation
 of Diphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7650
_journal_page_last               7662
_journal_paper_doi               10.1021/ic100816u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C43 H42 Cu F6 N P4'
_chemical_formula_weight         874.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.820(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.1600(11)
_cell_length_b                   14.0993(6)
_cell_length_c                   20.7714(8)
_cell_measurement_reflns_used    9373
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.74
_cell_measurement_theta_min      3.24
_cell_volume                     7982.2(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.919
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46319
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         65.22
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.811
_exptl_absorpt_correction_T_max  0.8064
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.901
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         12566
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0609P)^2^+12.8506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                10528
_reflns_number_total             12566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100816u_si_003_05.cif
_cod_data_source_block           glu305
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        7982.2(5)
_cod_database_code               4316385