#------------------------------------------------------------------------------
#$Date: 2016-03-21 12:56:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178689 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/00/4080011.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_4080011
loop_
_publ_author_name
'Béthegnies, Aurélien'
'Daran, Jean-Claude'
'Poli, Rinaldo'
_publ_section_title
;
 Platinum-Catalyzed Hydroamination of Ethylene: Study of the Catalyst
 Decomposition Mechanism
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              673
_journal_paper_doi               10.1021/om301182x
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C10 H10 Br2 N2 Pt'
_chemical_formula_sum            'C10 H10 Br2 N2 Pt'
_chemical_formula_weight         513.11
_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                 97.676(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.4963(4)
_cell_length_b                   17.4039(6)
_cell_length_c                   15.2525(6)
_cell_measurement_reflns_used    12760
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.9
_cell_volume                     2498.23(17)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_measurement_method       \wscan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12760
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    17.600
_exptl_absorpt_correction_T_max  0.0485
_exptl_absorpt_correction_T_min  0.0222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.049
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0353
_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)+(0.0738P)²+18.8889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                2527
_reflns_number_total             2752
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om301182x_si_001.cif
_cod_data_source_block           PtBr2(PhNH2)2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4080011
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.84302(3) 0.119668(14) 0.974903(18) 0.02720(13) Uani 1 1 d .
Br1 Br 0.89601(8) 0.07630(4) 1.12684(5) 0.03545(19) Uani 1 1 d .
Br2 Br 1.00019(9) 0.22806(5) 1.00304(6) 0.0400(2) Uani 1 1 d .
N1 N 0.8015(6) 0.1533(3) 0.8482(4) 0.0281(12) Uani 1 1 d .
N2 N 0.7082(6) 0.0309(3) 0.9436(4) 0.0299(12) Uani 1 1 d .
C11 C 0.8335(8) 0.1067(4) 0.7841(5) 0.0316(15) Uani 1 1 d .
H11 H 0.8735 0.0577 0.7996 0.038 Uiso 1 1 calc R
C12 C 0.8099(9) 0.1279(5) 0.6951(6) 0.0377(17) Uani 1 1 d .
H12 H 0.8342 0.0940 0.6506 0.045 Uiso 1 1 calc R
C13 C 0.7512(9) 0.1984(5) 0.6730(6) 0.0431(19) Uani 1 1 d .
H13 H 0.7359 0.2143 0.6129 0.052 Uiso 1 1 calc R
C14 C 0.7142(10) 0.2463(5) 0.7387(7) 0.0439(19) Uani 1 1 d .
H14 H 0.6707 0.2946 0.7243 0.053 Uiso 1 1 calc R
C15 C 0.7419(9) 0.2222(5) 0.8253(6) 0.0393(18) Uani 1 1 d .
H15 H 0.7182 0.2553 0.8707 0.047 Uiso 1 1 calc R
C21 C 0.5743(8) 0.0454(5) 0.9055(6) 0.0366(16) Uani 1 1 d .
H21 H 0.5432 0.0972 0.8982 0.044 Uiso 1 1 calc R
C22 C 0.4825(9) -0.0125(5) 0.8773(6) 0.0436(19) Uani 1 1 d .
H22 H 0.3884 -0.0012 0.8508 0.052 Uiso 1 1 calc R
C23 C 0.5272(10) -0.0872(5) 0.8874(6) 0.0430(19) Uani 1 1 d .
H23 H 0.4642 -0.1282 0.8687 0.052 Uiso 1 1 calc R
C24 C 0.6644(10) -0.1022(5) 0.9250(6) 0.0393(17) Uani 1 1 d .
H24 H 0.6981 -0.1536 0.9310 0.047 Uiso 1 1 calc R
C25 C 0.7522(8) -0.0417(4) 0.9536(6) 0.0345(16) Uani 1 1 d .
H25 H 0.8461 -0.0519 0.9811 0.041 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 0.02642(18) 0.02626(18) 0.0291(2) 0.00136(9) 0.00450(12) -0.00180(8)
Br1 0.0367(4) 0.0382(4) 0.0309(4) 0.0050(3) 0.0025(3) -0.0026(3)
Br2 0.0400(4) 0.0375(4) 0.0422(5) -0.0008(3) 0.0045(3) -0.0130(3)
N1 0.026(3) 0.029(3) 0.029(3) -0.003(2) 0.002(2) -0.003(2)
N2 0.028(3) 0.028(3) 0.035(3) 0.003(2) 0.008(2) -0.003(2)
C11 0.033(4) 0.030(3) 0.031(4) 0.002(3) 0.001(3) 0.002(3)
C12 0.043(4) 0.046(4) 0.024(4) -0.003(3) 0.004(3) 0.004(3)
C13 0.044(4) 0.047(5) 0.038(5) 0.004(4) 0.007(4) 0.004(4)
C14 0.049(5) 0.037(4) 0.046(5) 0.008(4) 0.011(4) 0.011(3)
C15 0.041(4) 0.033(4) 0.045(5) 0.007(3) 0.011(4) 0.008(3)
C21 0.031(3) 0.034(4) 0.045(5) 0.002(3) 0.005(3) -0.003(3)
C22 0.032(4) 0.051(5) 0.048(5) 0.007(4) 0.003(3) -0.006(3)
C23 0.052(5) 0.038(4) 0.038(5) -0.003(3) 0.005(4) -0.020(4)
C24 0.048(5) 0.031(3) 0.040(5) 0.000(3) 0.009(4) -0.003(3)
C25 0.033(4) 0.031(3) 0.041(4) 0.003(3) 0.011(3) 0.004(3)
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 N2 87.6(2)
N1 Pt1 Br2 88.89(16)
N2 Pt1 Br2 176.53(18)
N1 Pt1 Br1 178.61(17)
N2 Pt1 Br1 91.82(18)
Br2 Pt1 Br1 91.66(3)
C11 N1 C15 118.6(7)
C11 N1 Pt1 119.5(5)
C15 N1 Pt1 121.9(5)
C25 N2 C21 119.4(6)
C25 N2 Pt1 121.2(5)
C21 N2 Pt1 119.3(5)
N1 C11 C12 121.9(7)
C13 C12 C11 118.9(8)
C12 C13 C14 119.7(8)
C15 C14 C13 118.5(8)
N1 C15 C14 122.5(8)
N2 C21 C22 121.5(7)
C21 C22 C23 119.4(8)
C22 C23 C24 119.3(8)
C23 C24 C25 119.1(8)
N2 C25 C24 121.4(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pt1 N1 2.007(6)
Pt1 N2 2.023(6)
Pt1 Br2 2.4082(8)
Pt1 Br1 2.4253(8)
N1 C11 1.336(10)
N1 C15 1.352(10)
N2 C25 1.333(9)
N2 C21 1.350(10)
C11 C12 1.396(12)
C12 C13 1.371(12)
C13 C14 1.384(13)
C14 C15 1.378(13)
C21 C22 1.365(12)
C22 C23 1.369(13)
C23 C24 1.377(13)
C24 C25 1.378(11)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C13 H13 Br2 0.9500 2.8000 3.520(9) 134.00 8_455 yes
