#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:47:51 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178582 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/93/4069355.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_4069355
loop_
_publ_author_name
'Vicente, José'
'Arcas, Aurelia'
'Gálvez-López, María-Dolores'
'Jones, Peter G.'
'Bautista, Delia'
_publ_section_title
;
 Mono(2,6-dinitroaryl)platinum(II) and Mono- and
 Bis(2,6-dinitroaryl)platinum(IV) Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3501
_journal_paper_doi               10.1021/om9001582
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C16 H17 Br N2 O7 Pt'
_chemical_formula_weight         624.32
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 101.119(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6672(4)
_cell_length_b                   10.1737(8)
_cell_length_c                   14.2564(11)
_cell_measurement_reflns_used    6081
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      3.1
_cell_volume                     948.86(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'ω- & φ-scan'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19121
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    9.540
_exptl_absorpt_correction_T_max  0.7005
_exptl_absorpt_correction_T_min  0.0528
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.024
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment
'H at C2,C3 free with SADI, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2924
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0161
_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)+(0.0212P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0371
_refine_ls_wR_factor_ref         0.0377
_reflns_number_gt                2692
_reflns_number_total             2924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9001582_si_002.cif
_cod_data_source_block           plath
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4069355
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z'
'-x, -y, -z'
'-x, y-1/2, -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
Pt Pt 0.352646(14) 0.2500 0.408628(7) 0.01543(4) Uani 1 2 d S
Br Br 0.63879(4) 0.2500 0.32754(2) 0.02548(7) Uani 1 2 d S
N1 N 0.1468(2) 0.00709(16) 0.27490(12) 0.0192(3) Uani 1 1 d .
O1 O 0.0596(3) -0.03879(16) 0.33607(13) 0.0330(4) Uani 1 1 d .
O2 O 0.2874(2) -0.04606(16) 0.24707(12) 0.0336(4) Uani 1 1 d .
O3 O -0.1319(2) 0.01242(14) 0.10940(11) 0.0235(3) Uani 1 1 d .
O4 O -0.2854(3) 0.2500 0.02271(15) 0.0233(4) Uani 1 2 d S
C1 C 0.3220(3) 0.13859(19) 0.58713(14) 0.0212(4) Uani 1 1 d .
H1 H 0.3173 0.0460 0.6103 0.025 Uiso 1 1 calc R
C2 C 0.5176(3) 0.1828(2) 0.55364(14) 0.0216(4) Uani 1 1 d D
H2 H 0.633(3) 0.128(2) 0.5472(19) 0.033(7) Uiso 1 1 d D
C3 C 0.1539(3) 0.1815(2) 0.50182(15) 0.0214(4) Uani 1 1 d D
H3 H 0.043(3) 0.124(2) 0.4713(17) 0.030(7) Uiso 1 1 d D
C4 C 0.3043(5) 0.2500 0.6590(2) 0.0239(6) Uani 1 2 d S
H4A H 0.4183 0.2500 0.7150 0.029 Uiso 1 2 calc SR
H4B H 0.1714 0.2500 0.6802 0.029 Uiso 1 2 calc SR
C11 C 0.1536(4) 0.2500 0.2811(2) 0.0170(5) Uani 1 2 d S
C12 C 0.0760(3) 0.13636(19) 0.23312(14) 0.0170(4) Uani 1 1 d .
C13 C -0.0680(3) 0.13216(19) 0.14884(14) 0.0180(4) Uani 1 1 d .
C14 C -0.1409(4) 0.2500 0.1053(2) 0.0188(5) Uani 1 2 d S
C15 C -0.3355(3) -0.0226(2) 0.1216(2) 0.0330(5) Uani 1 1 d .
H15A H -0.3357 -0.0356 0.1897 0.040 Uiso 1 1 calc R
H15B H -0.3780 -0.1040 0.0867 0.040 Uiso 1 1 calc R
H15C H -0.4307 0.0482 0.0967 0.040 Uiso 1 1 calc R
C16 C -0.1947(6) 0.2500 -0.0610(2) 0.0342(8) Uani 1 2 d S
H16A H -0.3028 0.2500 -0.1184 0.041 Uiso 1 2 d SR
H16B H -0.1098 0.1713 -0.0609 0.041 Uiso 1 1 d 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.020
0.00 0.00 1.00 0.018
0.00 -1.00 0.00 0.078
0.00 1.00 0.00 0.086
2.00 0.00 -1.00 0.168
-1.00 -1.00 0.00 0.174
-1.00 1.00 0.00 0.180
-1.00 0.00 -2.00 0.127
-1.00 0.00 2.00 0.132
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
C11 Pt C3 100.23(9) . 2
C11 Pt C3 100.23(9) . .
C3 Pt C3 37.56(11) 2 .
C11 Pt C2 159.96(7) . 2
C3 Pt C2 65.63(8) 2 2
C3 Pt C2 77.45(8) . 2
C11 Pt C2 159.96(7) . .
C3 Pt C2 77.45(8) 2 .
C3 Pt C2 65.63(8) . .
C2 Pt C2 35.32(11) 2 .
C11 Pt Br 90.66(8) . .
C3 Pt Br 158.10(6) 2 .
C3 Pt Br 158.10(5) . .
C2 Pt Br 98.54(6) 2 .
C2 Pt Br 98.54(6) . .
O2 N1 O1 124.30(18) . .
O2 N1 C12 118.03(18) . .
O1 N1 C12 117.67(17) . .
C13 O3 C15 113.14(17) . .
C14 O4 C16 112.0(2) . .
C2 C1 C4 99.70(17) . .
C2 C1 C3 101.65(16) . .
C4 C1 C3 100.21(17) . .
C2 C2 C1 107.00(11) 2 .
C2 C2 Pt 72.34(5) 2 .
C1 C2 Pt 94.63(11) . .
C3 C3 C1 106.37(11) 2 .
C3 C3 Pt 71.22(6) 2 .
C1 C3 Pt 97.85(13) . .
C1 C4 C1 94.2(2) . 2
C12 C11 C12 112.4(2) . 2
C12 C11 Pt 123.79(12) . .
C12 C11 Pt 123.79(12) 2 .
C13 C12 C11 125.55(18) . .
C13 C12 N1 115.74(16) . .
C11 C12 N1 118.70(17) . .
O3 C13 C12 119.34(17) . .
O3 C13 C14 121.78(17) . .
C12 C13 C14 118.88(18) . .
O4 C14 C13 120.63(12) . 2
O4 C14 C13 120.63(12) . .
C13 C14 C13 118.7(2) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt C11 2.034(3) .
Pt C3 2.165(2) 2
Pt C3 2.165(2) .
Pt C2 2.252(2) 2
Pt C2 2.252(2) .
Pt Br 2.4138(3) .
N1 O2 1.213(2) .
N1 O1 1.229(2) .
N1 C12 1.483(2) .
O3 C13 1.374(2) .
O3 C15 1.446(3) .
O4 C14 1.370(3) .
O4 C16 1.438(4) .
C1 C2 1.540(3) .
C1 C4 1.548(3) .
C1 C3 1.550(3) .
C2 C2 1.367(4) 2
C3 C3 1.394(4) 2
C4 C1 1.548(3) 2
C11 C12 1.391(2) .
C11 C12 1.391(2) 2
C12 C13 1.387(3) .
C13 C14 1.394(2) .
C14 C13 1.394(2) 2
