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_4316389
_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_moiety         'C54 H51 Cl Cu P4, C2 H6 O, F6 P'
_chemical_formula_sum            'C56 H57 Cl Cu F6 O P5'
_chemical_formula_weight         1113.86
_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                 100.073(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.627(2)
_cell_length_b                   25.660(5)
_cell_length_c                   19.383(4)
_cell_measurement_reflns_used    2010
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.01
_cell_measurement_theta_min      2.28
_cell_volume                     5204.1(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1151
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46550
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.9222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         10736
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                6292
_reflns_number_total             10736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100816u_si_003_09.cif
_cod_data_source_block           glu322
_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        5204.0(19)
_cod_database_code               4316389