#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:50:34 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178584 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/95/4069531.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4069531
loop_
_publ_author_name
'Dub, Pavel A.'
'Rodriguez-Zubiri, Mireia'
'Daran, Jean-Claude'
'Brunet, Jean-Jacques'
'Poli, Rinaldo'
_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         'C16 H36 P, 0.5( Br6 Pt2)'
_chemical_formula_sum            'C16 H36 Br3 P Pt'
_chemical_formula_weight         694.24
_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                 91.273(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5046(3)
_cell_length_b                   17.7168(5)
_cell_length_c                   13.5383(4)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.34
_cell_measurement_theta_min      2.65
_cell_volume                     2279.17(12)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_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., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector, APEXII'
_diffrn_measurement_method       'φ and ω 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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            67188
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    11.481
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.396
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         6131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0300
_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/[σ²(Fo²)+(0.0470P)²+2.2543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                4695
_reflns_number_total             6131
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om9002494_si_002.cif
_cod_data_source_block           1'
_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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               4069531
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pt1 Pt 0.896659(19) 0.083002(11) 0.475578(15) 0.03052(7) Uani 1 1 d .
Br1 Br 0.87289(6) 0.20373(3) 0.55689(5) 0.04161(14) Uani 1 1 d .
Br2 Br 0.73327(6) 0.11717(4) 0.34456(5) 0.04659(15) Uani 1 1 d .
Br3 Br 0.93825(6) -0.03847(3) 0.39642(4) 0.03831(13) Uani 1 1 d .
P1 P 0.30643(13) 0.21948(8) 0.41671(10) 0.0297(3) Uani 1 1 d .
C111 C 0.3727(6) 0.1353(3) 0.4757(4) 0.0352(12) Uani 1 1 d .
H11A H 0.2914 0.1031 0.4922 0.042 Uiso 1 1 calc R
H11B H 0.4291 0.1073 0.4272 0.042 Uiso 1 1 calc R
C112 C 0.4628(6) 0.1462(3) 0.5693(4) 0.0411(8) Uani 1 1 d .
H11C H 0.5429 0.1798 0.5547 0.049 Uiso 1 1 calc R
H11D H 0.4058 0.1709 0.6204 0.049 Uiso 1 1 calc R
C113 C 0.5183(7) 0.0723(3) 0.6088(4) 0.0411(8) Uani 1 1 d .
H11E H 0.5775 0.0484 0.5583 0.049 Uiso 1 1 calc R
H11F H 0.4381 0.0381 0.6210 0.049 Uiso 1 1 calc R
C114 C 0.6049(6) 0.0814(3) 0.7043(4) 0.0411(8) Uani 1 1 d .
H11G H 0.6910 0.1096 0.6908 0.062 Uiso 1 1 calc R
H11H H 0.6296 0.0315 0.7307 0.062 Uiso 1 1 calc R
H11I H 0.5496 0.1090 0.7528 0.062 Uiso 1 1 calc R
C121 C 0.4396(5) 0.2616(3) 0.3429(4) 0.0372(12) Uani 1 1 d .
H12A H 0.4859 0.2209 0.3055 0.045 Uiso 1 1 calc R
H12B H 0.3927 0.2954 0.2942 0.045 Uiso 1 1 calc R
C122 C 0.5535(6) 0.3067(3) 0.3973(5) 0.0403(13) Uani 1 1 d .
H12C H 0.6049 0.2737 0.4448 0.048 Uiso 1 1 calc R
H12D H 0.5102 0.3484 0.4346 0.048 Uiso 1 1 calc R
C123 C 0.6559(8) 0.3388(5) 0.3222(6) 0.066(2) Uani 1 1 d .
H12E H 0.7052 0.2964 0.2902 0.079 Uiso 1 1 calc R
H12F H 0.6015 0.3661 0.2703 0.079 Uiso 1 1 calc R
C124 C 0.7598(9) 0.3896(6) 0.3652(8) 0.087(3) Uani 1 1 d .
H12G H 0.7134 0.4255 0.4089 0.130 Uiso 1 1 calc R
H12H H 0.8066 0.4172 0.3125 0.130 Uiso 1 1 calc R
H12I H 0.8298 0.3605 0.4034 0.130 Uiso 1 1 calc R
C131 C 0.2456(6) 0.2840(3) 0.5084(4) 0.0339(11) Uani 1 1 d .
H13A H 0.1740 0.2585 0.5485 0.041 Uiso 1 1 calc R
H13B H 0.3255 0.2978 0.5530 0.041 Uiso 1 1 calc R
C132 C 0.1819(7) 0.3562(4) 0.4643(5) 0.0484(9) Uani 1 1 d .
H13C H 0.2475 0.3771 0.4156 0.058 Uiso 1 1 calc R
H13D H 0.0931 0.3433 0.4285 0.058 Uiso 1 1 calc R
C133 C 0.1513(7) 0.4168(4) 0.5411(5) 0.0484(9) Uani 1 1 d .
H13E H 0.2383 0.4264 0.5807 0.058 Uiso 1 1 calc R
H13F H 0.1258 0.4642 0.5064 0.058 Uiso 1 1 calc R
C134 C 0.0362(7) 0.3968(4) 0.6095(5) 0.0484(9) Uani 1 1 d .
H13G H -0.0523 0.3908 0.5717 0.073 Uiso 1 1 calc R
H13H H 0.0258 0.4370 0.6585 0.073 Uiso 1 1 calc R
H13I H 0.0593 0.3493 0.6433 0.073 Uiso 1 1 calc R
C141 C 0.1637(5) 0.1958(3) 0.3333(4) 0.0366(12) Uani 1 1 d .
H14A H 0.0787 0.1859 0.3723 0.044 Uiso 1 1 calc R
H14B H 0.1435 0.2398 0.2903 0.044 Uiso 1 1 calc R
C142 C 0.1913(6) 0.1273(4) 0.2682(4) 0.0421(13) Uani 1 1 d .
H14C H 0.2851 0.1326 0.2387 0.051 Uiso 1 1 calc R
H14D H 0.1925 0.0813 0.3097 0.051 Uiso 1 1 calc R
C143 C 0.0816(6) 0.1184(4) 0.1867(4) 0.0482(15) Uani 1 1 d .
H14E H 0.0888 0.1614 0.1405 0.058 Uiso 1 1 calc R
H14F H -0.0130 0.1199 0.2157 0.058 Uiso 1 1 calc R
C144 C 0.0973(8) 0.0451(4) 0.1294(5) 0.0604(19) Uani 1 1 d .
H14G H 0.1932 0.0413 0.1048 0.091 Uiso 1 1 calc R
H14H H 0.0300 0.0445 0.0735 0.091 Uiso 1 1 calc R
H14I H 0.0787 0.0022 0.1729 0.091 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
Br2 Pt1 Br1 92.74(2) .
Br2 Pt1 Br3 90.36(2) .
Br1 Pt1 Br3 175.98(2) .
Br2 Pt1 Br3 175.61(2) 3_756
Br1 Pt1 Br3 91.59(2) 3_756
Br3 Pt1 Br3 85.350(19) 3_756
Pt1 Br3 Pt1 94.650(19) 3_756
C121 P1 C131 111.3(3) .
C121 P1 C141 106.3(3) .
C131 P1 C141 109.5(2) .
C121 P1 C111 110.4(3) .
C131 P1 C111 109.7(3) .
C141 P1 C111 109.7(3) .
C112 C111 P1 116.6(4) .
C113 C112 C111 111.7(5) .
C112 C113 C114 112.7(5) .
C122 C121 P1 116.9(4) .
C121 C122 C123 109.2(5) .
C124 C123 C122 113.7(7) .
C132 C131 P1 113.2(4) .
C133 C132 C131 113.6(5) .
C134 C133 C132 114.2(6) .
C142 C141 P1 114.3(4) .
C143 C142 C141 112.4(5) .
C142 C143 C144 112.9(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 Br2 2.4087(6) .
Pt1 Br1 2.4184(6) .
Pt1 Br3 2.4403(6) .
Pt1 Br3 2.4427(6) 3_756
Br3 Pt1 2.4427(6) 3_756
P1 C121 1.792(5) .
P1 C131 1.793(5) .
P1 C141 1.795(5) .
P1 C111 1.799(6) .
C111 C112 1.527(8) .
C112 C113 1.505(8) .
C113 C114 1.526(8) .
C121 C122 1.522(8) .
C122 C123 1.532(9) .
C123 C124 1.450(11) .
C131 C132 1.531(8) .
C132 C133 1.527(9) .
C133 C134 1.492(9) .
C141 C142 1.525(8) .
C142 C143 1.509(8) .
C143 C144 1.522(9) .
