Platinum-Catalyzed Ethylene Hydroamination with Aniline: Synthesis, Characterization, and Studies of Intermediates
Dub, Pavel A.; Rodriguez-Zubiri, Mireia; Daran, Jean-Claude; Brunet, Jean-Jacques; Poli, Rinaldo; Organometallics 28 (2009) 4764–; doi:10.1021/om9002494

data_4069530
_publ_section_title
;
 Platinum-Catalyzed Ethylene Hydroamination with Aniline: Synthesis,
 Characterization, and Studies of Intermediates
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4764
_journal_paper_doi               10.1021/om9002494
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         '2(C16 H36 P), Br4 Pt'
_chemical_formula_sum            'C32 H72 Br4 P2 Pt'
_chemical_formula_weight         1033.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 120.783(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.824(2)
_cell_length_b                   12.4983(6)
_cell_length_c                   24.4141(12)
_cell_measurement_reflns_used    10818
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.19
_cell_measurement_theta_min      2.61
_cell_volume                     8342.5(9)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            33681
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    7.291
_exptl_absorpt_correction_T_max  0.173
_exptl_absorpt_correction_T_min  0.131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm within
CrysAlis RED (Oxford Diffraction, 2007)
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.227
_refine_diff_density_max         2.113
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9186
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0508P)^2^+99.7750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                5440
_reflns_number_total             9186
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om9002494_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        8342.5(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4069530