Investigation of Steric and Electronic Features of 3-Iminophosphine-Based Palladium Catalysts for Intermolecular Hydroamination
Zingales, Nicholas C.; Shaffer, Andrew R.; Schmidt, Joseph A. R.; Organometallics 32 (2013) 578–; doi:10.1021/om301102w

data_4079960
_publ_section_title
;
 Investigation of Steric and Electronic Features of 3-Iminophosphine-Based
 Palladium Catalysts for Intermolecular Hydroamination
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              578
_journal_paper_doi               10.1021/om301102w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C30 H31 F3 N O3 P Pd S'
_chemical_formula_weight         679.99
_chemical_name_common            1Pd
_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                 98.402(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.331(4)
_cell_length_b                   9.6895(17)
_cell_length_c                   28.509(5)
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      56.84
_cell_volume                     5829.2(18)
_computing_cell_refinement       'Bruker SAINT v6.22'
_computing_data_collection       'Bruker SMART v5.625'
_computing_data_reduction        'Bruker SAINT v6.622'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  SMART
_diffrn_measurement_method       \w-scan
_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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            64333
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.788192
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.709
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         14493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.140
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+4.7964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                11637
_reflns_number_total             14493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301102w_si_003.cif
_cod_data_source_block           1Pd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        5829.3(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4079960