#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/95/4069535.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_4069535
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         'C8 H11 Br2 N Pt'
_chemical_formula_sum            'C8 H11 Br2 N Pt'
_chemical_formula_weight         476.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6706(3)
_cell_length_b                   9.6392(2)
_cell_length_c                   17.7660(4)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      38.53
_cell_measurement_theta_min      2.29
_cell_volume                     2169.84(8)
_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         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34000
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    20.248
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.915
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flattened needle'
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.007
_refine_diff_density_max         3.385
_refine_diff_density_min         -3.681
_refine_diff_density_rms         0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1156P)²+51.0719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                2234
_reflns_number_total             2690
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om9002494_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_Hall     '-P 2ac 2ab '
_cod_original_sg_symbol_H-M      'Pbca '
_cod_database_code               4069535
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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 0.10777(3) 0.09853(4) 0.68679(2) 0.0171(2) Uani 1 1 d .
Br1 Br 0.04092(11) 0.33382(13) 0.69345(7) 0.0284(3) Uani 1 1 d .
Br2 Br 0.21191(12) 0.13403(15) 0.80045(8) 0.0310(3) Uani 1 1 d .
N1 N 0.1726(9) -0.1000(10) 0.6863(6) 0.023(2) Uani 1 1 d .
H1A H 0.2418 -0.0908 0.6965 0.027 Uiso 1 1 calc R
H1B H 0.1438 -0.1462 0.7252 0.027 Uiso 1 1 calc R
C1 C 0.0528(11) 0.0903(13) 0.5747(8) 0.028(3) Uani 1 1 d .
H1C H 0.0381 0.1786 0.5507 0.034 Uiso 1 1 calc R
H1D H 0.0876 0.0244 0.5417 0.034 Uiso 1 1 calc R
C2 C -0.0245(10) 0.0384(14) 0.6204(6) 0.025(3) Uani 1 1 d .
H2A H -0.0383 -0.0603 0.6166 0.030 Uiso 1 1 calc R
H2B H -0.0879 0.0941 0.6256 0.030 Uiso 1 1 calc R
C11 C 0.1639(9) -0.1896(12) 0.6205(8) 0.024(2) Uani 1 1 d .
C12 C 0.2340(10) -0.1709(14) 0.5617(7) 0.029(3) Uani 1 1 d .
H12 H 0.2879 -0.1057 0.5652 0.034 Uiso 1 1 calc R
C13 C 0.2223(12) -0.2532(17) 0.4959(8) 0.038(3) Uani 1 1 d .
H13 H 0.2674 -0.2407 0.4551 0.046 Uiso 1 1 calc R
C14 C 0.1446(14) -0.3502(14) 0.4931(9) 0.039(4) Uani 1 1 d .
H14 H 0.1371 -0.4053 0.4505 0.046 Uiso 1 1 calc R
C15 C 0.0754(13) -0.3679(15) 0.5543(9) 0.038(3) Uani 1 1 d .
H15 H 0.0225 -0.4346 0.5522 0.045 Uiso 1 1 calc R
C16 C 0.0862(11) -0.2876(13) 0.6163(7) 0.028(3) Uani 1 1 d .
H16 H 0.0402 -0.2992 0.6566 0.034 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0156(3) 0.0170(3) 0.0187(3) -0.00102(14) -0.00056(15) -0.00037(14)
Br1 0.0318(7) 0.0209(6) 0.0325(7) -0.0012(5) 0.0052(5) 0.0061(5)
Br2 0.0341(7) 0.0335(7) 0.0255(6) -0.0057(5) -0.0107(5) -0.0014(6)
N1 0.020(5) 0.017(5) 0.031(6) 0.000(4) -0.008(4) 0.000(4)
C1 0.026(7) 0.030(6) 0.028(7) -0.001(5) -0.007(5) 0.010(5)
C2 0.027(6) 0.040(7) 0.007(5) -0.001(5) 0.002(4) 0.003(5)
C11 0.019(6) 0.016(5) 0.036(7) -0.003(5) -0.001(5) 0.010(4)
C12 0.024(6) 0.036(7) 0.026(6) -0.002(5) -0.002(5) 0.002(5)
C13 0.039(9) 0.049(8) 0.025(6) 0.011(6) 0.006(6) 0.019(7)
C14 0.055(10) 0.029(7) 0.032(8) -0.005(6) -0.021(7) 0.013(7)
C15 0.047(8) 0.031(7) 0.035(8) -0.011(6) 0.004(7) -0.008(7)
C16 0.038(7) 0.023(6) 0.023(6) -0.003(5) 0.011(5) 0.001(5)
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'
N N 0.0061 0.0033 '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
N1 Pt1 C1 95.3(4)
N1 Pt1 C2 93.3(5)
C1 Pt1 C2 37.6(5)
N1 Pt1 Br1 176.2(3)
C1 Pt1 Br1 88.0(3)
C2 Pt1 Br1 90.4(4)
N1 Pt1 Br2 85.4(3)
C1 Pt1 Br2 165.0(4)
C2 Pt1 Br2 157.4(3)
Br1 Pt1 Br2 91.00(5)
C11 N1 Pt1 121.2(8)
C2 C1 Pt1 71.9(8)
C1 C2 Pt1 70.5(8)
C16 C11 C12 120.8(12)
C16 C11 N1 120.5(11)
C12 C11 N1 118.7(11)
C11 C12 C13 118.8(13)
C14 C13 C12 119.3(14)
C13 C14 C15 120.5(13)
C16 C15 C14 119.8(14)
C15 C16 C11 120.8(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 N1 2.082(10)
Pt1 C1 2.112(13)
Pt1 C2 2.130(12)
Pt1 Br1 2.4239(13)
Pt1 Br2 2.4364(13)
N1 C11 1.458(15)
C1 C2 1.367(18)
C11 C16 1.366(18)
C11 C12 1.383(18)
C12 C13 1.42(2)
C13 C14 1.36(2)
C14 C15 1.41(2)
C15 C16 1.354(19)
