#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:48:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178668 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/79/4077995.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_4077995
loop_
_publ_author_name
'Dub, Pavel A.'
'Béthegnies, Aurélien'
'Daran, Jean-Claude'
'Poli, Rinaldo'
_publ_section_title
;
 Formation and Structure of a Platinum(II) Complex Containing
 TwotransNonstabilized Phosphorus Ylide Ligands: Evidence for Reversible
 Ylide Dissociation
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3081
_journal_paper_doi               10.1021/om2012453
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H70 Br2 P2 Pt'
_chemical_formula_sum            'C32 H70 Br2 P2 Pt'
_chemical_formula_weight         871.70
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-11-14 # Formatted by publCIF
;
_cell_angle_alpha                99.468(3)
_cell_angle_beta                 94.966(3)
_cell_angle_gamma                101.819(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5724(5)
_cell_length_b                   9.8981(6)
_cell_length_c                   10.3109(5)
_cell_measurement_reflns_used    8308
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36.67
_cell_measurement_theta_min      2.19
_cell_volume                     935.86(9)
_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, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7913
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    5.987
_exptl_absorpt_correction_T_max  0.541
_exptl_absorpt_correction_T_min  0.053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flattened
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         5.253
_refine_diff_density_min         -3.364
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0566P)²+23.7667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                3007
_reflns_number_total             3490
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om2012453_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4077995
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C11 C 0.6513(11) 0.3859(13) 0.4225(10) 0.0223(2) Uani 1 1 d .
H11 H 0.5923 0.3004 0.3660 0.027 Uiso 1 1 calc R
C12 C 0.7533(14) 0.4496(15) 0.3352(13) 0.035(3) Uani 1 1 d .
H12A H 0.8105 0.3832 0.3044 0.042 Uiso 1 1 calc R
H12B H 0.8183 0.5330 0.3868 0.042 Uiso 1 1 calc R
C13 C 0.6768(15) 0.4892(17) 0.2151(12) 0.039(3) Uani 1 1 d .
H13A H 0.6159 0.5518 0.2462 0.047 Uiso 1 1 calc R
H13B H 0.7485 0.5405 0.1695 0.047 Uiso 1 1 calc R
C14 C 0.5871(17) 0.367(2) 0.1187(16) 0.060(5) Uani 1 1 d .
H14A H 0.6449 0.3011 0.0918 0.090 Uiso 1 1 calc R
H14B H 0.5500 0.3987 0.0425 0.090 Uiso 1 1 calc R
H14C H 0.5086 0.3220 0.1598 0.090 Uiso 1 1 calc R
C21 C 0.8422(11) 0.4676(14) 0.6819(11) 0.027(3) Uani 1 1 d .
H21A H 0.9258 0.4393 0.7191 0.032 Uiso 1 1 calc R
H21B H 0.8766 0.5480 0.6415 0.032 Uiso 1 1 calc R
C22 C 0.7588(13) 0.5144(14) 0.7958(12) 0.029(3) Uani 1 1 d .
H22A H 0.6623 0.5156 0.7593 0.035 Uiso 1 1 calc R
H22B H 0.7507 0.4462 0.8539 0.035 Uiso 1 1 calc R
C23 C 0.8299(15) 0.6593(16) 0.8770(14) 0.041(3) Uani 1 1 d .
H23A H 0.8322 0.7275 0.8191 0.050 Uiso 1 1 calc R
H23B H 0.7698 0.6826 0.9446 0.050 Uiso 1 1 calc R
C24 C 0.9808(17) 0.676(2) 0.9439(17) 0.065(5) Uani 1 1 d .
H24A H 0.9772 0.6307 1.0197 0.097 Uiso 1 1 calc R
H24B H 1.0249 0.7736 0.9717 0.097 Uiso 1 1 calc R
H24C H 1.0362 0.6326 0.8827 0.097 Uiso 1 1 calc R
C31 C 0.8748(12) 0.2322(13) 0.4927(11) 0.027(3) Uani 1 1 d .
H31A H 0.9438 0.2948 0.4538 0.033 Uiso 1 1 calc R
H31B H 0.9265 0.2073 0.5671 0.033 Uiso 1 1 calc R
C32 C 0.8118(13) 0.0994(16) 0.3902(13) 0.036(3) Uani 1 1 d .
H32A H 0.7550 0.0306 0.4329 0.043 Uiso 1 1 calc R
H32B H 0.7476 0.1214 0.3226 0.043 Uiso 1 1 calc R
C33 C 0.9242(15) 0.0350(17) 0.3243(14) 0.042(3) Uani 1 1 d .
H33A H 0.9953 0.0237 0.3922 0.051 Uiso 1 1 calc R
H33B H 0.9729 0.0989 0.2721 0.051 Uiso 1 1 calc R
C34 C 0.8613(19) -0.1070(18) 0.2348(15) 0.054(4) Uani 1 1 d .
H34A H 0.8181 -0.1725 0.2868 0.081 Uiso 1 1 calc R
H34B H 0.9365 -0.1411 0.1932 0.081 Uiso 1 1 calc R
H34C H 0.7897 -0.0969 0.1681 0.081 Uiso 1 1 calc R
C41 C 0.6233(12) 0.2058(14) 0.6302(11) 0.028(3) Uani 1 1 d .
H41A H 0.5583 0.2559 0.6743 0.033 Uiso 1 1 calc R
H41B H 0.5657 0.1318 0.5613 0.033 Uiso 1 1 calc R
C42 C 0.6985(13) 0.1384(14) 0.7308(12) 0.030(3) Uani 1 1 d .
H42A H 0.7528 0.0773 0.6846 0.035 Uiso 1 1 calc R
H42B H 0.7663 0.2118 0.7930 0.035 Uiso 1 1 calc R
C43 C 0.5973(14) 0.0547(15) 0.8069(13) 0.035(3) Uani 1 1 d .
H43A H 0.5354 -0.0240 0.7457 0.043 Uiso 1 1 calc R
H43B H 0.5367 0.1133 0.8465 0.043 Uiso 1 1 calc R
C44 C 0.6733(17) -0.0006(17) 0.9150(15) 0.048(4) Uani 1 1 d .
H44A H 0.7430 -0.0483 0.8788 0.072 Uiso 1 1 calc R
H44B H 0.6042 -0.0649 0.9504 0.072 Uiso 1 1 calc R
H44C H 0.7208 0.0764 0.9844 0.072 Uiso 1 1 calc R
P1 P 0.7423(3) 0.3256(3) 0.5537(3) 0.0211(6) Uani 1 1 d .
Br1 Br 0.31993(11) 0.27685(12) 0.45666(11) 0.0257(3) Uani 1 1 d .
Pt1 Pt 0.5000 0.5000 0.5000 0.0223(2) Uani 1 2 d S
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_1
_geom_angle_site_symmetry_3
C12 C11 P1 112.1(7) . .
C12 C11 Pt1 119.0(8) . .
P1 C11 Pt1 109.7(5) . .
C11 C12 C13 113.0(10) . .
C14 C13 C12 114.1(13) . .
C22 C21 P1 115.7(8) . .
C23 C22 C21 113.1(11) . .
C24 C23 C22 116.1(13) . .
C32 C31 P1 114.1(8) . .
C33 C32 C31 113.6(11) . .
C32 C33 C34 113.0(12) . .
C42 C41 P1 114.8(8) . .
C43 C42 C41 113.8(10) . .
C42 C43 C44 113.5(11) . .
C11 P1 C41 113.2(5) . .
C11 P1 C21 112.8(6) . .
C41 P1 C21 108.1(6) . .
C11 P1 C31 111.1(5) . .
C41 P1 C31 106.1(6) . .
C21 P1 C31 105.0(5) . .
C11 Pt1 C11 180.000(2) 2_666 .
C11 Pt1 Br1 91.9(3) 2_666 .
C11 Pt1 Br1 88.1(3) . .
C11 Pt1 Br1 88.1(3) 2_666 2_666
C11 Pt1 Br1 91.9(3) . 2_666
Br1 Pt1 Br1 180.0 . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C11 C12 1.499(17) .
C11 P1 1.794(10) .
C11 Pt1 2.141(11) .
C12 C13 1.531(17) .
C13 C14 1.49(2) .
C21 C22 1.538(16) .
C21 P1 1.805(12) .
C22 C23 1.526(19) .
C23 C24 1.51(2) .
C31 C32 1.523(18) .
C31 P1 1.813(12) .
C32 C33 1.514(18) .
C33 C34 1.52(2) .
C41 C42 1.527(15) .
C41 P1 1.799(12) .
C42 C43 1.502(17) .
C43 C44 1.515(17) .
Br1 Pt1 2.4560(11) .
Pt1 C11 2.141(11) 2_666
Pt1 Br1 2.4560(11) 2_666
