#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:52:43 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180100 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/46/7054686.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_7054686
loop_
_publ_author_name
'Ghosh, Biswa Nath'
'Lentz, Dieter'
'Schlecht, Sabine'
_publ_section_title
;
 Substituent effects in solution speciation of the mononuclear and
 dinuclear trimethylplatinum(iv) iodide complexes of pyridines
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              3536
_journal_paper_doi               10.1039/C4NJ02426E
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C20 H36 I2 N2 Pt2'
_chemical_formula_sum            'C20 H36 I2 N2 Pt2'
_chemical_formula_weight         948.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2c 2n'
_space_group_name_H-M_alt        'P n a m'
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-12-29 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7003(10)
_cell_length_b                   12.7871(9)
_cell_length_c                   18.4091(17)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.45
_cell_volume                     2518.8(4)
_computing_cell_refinement       'STOE IPDS Software (1997)'
_computing_data_collection       'STOE IPDS Software (1997)'
_computing_data_reduction        'STOE IPDS Software (1997)'
_computing_molecular_graphics    'Mercury v3.3 (Macrae et al., 2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution
;
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
;
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi 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  0.0646
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16248
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.326
_exptl_absorpt_coefficient_mu    13.554
_exptl_absorpt_correction_T_max  0.1480
_exptl_absorpt_correction_T_min  0.0562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.340
_refine_diff_density_min         -2.403
_refine_diff_density_rms         0.283
_refine_ls_extinction_coef       0.00201(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0735P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2023
_reflns_number_total             2215
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4nj02426e2.cif
_cod_data_source_block           syn-[PtMe3(4-Etpy)I]2
_cod_depositor_comments
'Adding full bibliography for 7054680--7054686.cif.'
_cod_database_code               7054686
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.091
_shelx_estimated_absorpt_t_max   0.220
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pt1 Pt 0.15483(2) 0.06646(2) 0.36006(2) 0.02444(17) Uani 1 1 d . . .
I1 I 0.23231(5) -0.07213(5) 0.2500 0.0288(2) Uani 1 2 d S T P
I2 I 0.10711(6) 0.20968(5) 0.2500 0.0288(2) Uani 1 2 d S T P
N1 N -0.0365(5) 0.0067(5) 0.3527(3) 0.0264(13) Uani 1 1 d . . .
C1 C 0.3345(7) 0.1209(7) 0.3700(4) 0.0381(19) Uani 1 1 d . . .
H1A H 0.3373 0.1757 0.4072 0.062(7) Uiso 1 1 calc R U .
H1B H 0.3623 0.1498 0.3234 0.062(7) Uiso 1 1 calc R U .
H1C H 0.3897 0.0633 0.3842 0.062(7) Uiso 1 1 calc R U .
C2 C 0.1918(8) -0.0344(7) 0.4427(4) 0.0427(18) Uani 1 1 d . . .
H2A H 0.2553 -0.0040 0.4747 0.062(7) Uiso 1 1 calc R U .
H2B H 0.2227 -0.1006 0.4227 0.062(7) Uiso 1 1 calc R U .
H2C H 0.1152 -0.0472 0.4704 0.062(7) Uiso 1 1 calc R U .
C3 C 0.1031(8) 0.1698(7) 0.4407(4) 0.0440(19) Uani 1 1 d . . .
H3A H 0.1653 0.1683 0.4798 0.062(7) Uiso 1 1 calc R U .
H3B H 0.0213 0.1496 0.4601 0.062(7) Uiso 1 1 calc R U .
H3C H 0.0982 0.2406 0.4205 0.062(7) Uiso 1 1 calc R U .
C4 C -0.1382(7) 0.0694(6) 0.3502(5) 0.0359(19) Uani 1 1 d . . .
H4 H -0.1260 0.1430 0.3491 0.062(7) Uiso 1 1 calc R U .
C5 C -0.2580(7) 0.0316(6) 0.3492(4) 0.0332(15) Uani 1 1 d . . .
H5 H -0.3259 0.0794 0.3484 0.062(7) Uiso 1 1 calc R U .
C6 C -0.2818(7) -0.0733(5) 0.3493(4) 0.0266(15) Uani 1 1 d . . .
C7 C -0.1774(7) -0.1392(6) 0.3503(4) 0.0333(16) Uani 1 1 d . . .
H7 H -0.1877 -0.2130 0.3496 0.062(7) Uiso 1 1 calc R U .
C8 C -0.0591(7) -0.0958(6) 0.3524(4) 0.0327(16) Uani 1 1 d . . .
H8 H 0.0104 -0.1419 0.3537 0.062(7) Uiso 1 1 calc R U .
C9 C -0.4109(7) -0.1195(8) 0.3504(4) 0.0392(18) Uani 1 1 d . . .
H9A H -0.4114 -0.1856 0.3224 0.062(7) Uiso 1 1 calc R U .
H9B H -0.4701 -0.0705 0.3270 0.062(7) Uiso 1 1 calc R U .
C10 C -0.4531(7) -0.1409(7) 0.4275(4) 0.0438(19) Uani 1 1 d . . .
H10A H -0.4052 -0.1996 0.4474 0.062(7) Uiso 1 1 calc R U .
H10B H -0.5423 -0.1585 0.4276 0.062(7) Uiso 1 1 calc R U .
H10C H -0.4392 -0.0786 0.4574 0.062(7) Uiso 1 1 calc R U .
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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
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
C2 Pt1 C1 88.1(3) . .
C2 Pt1 C3 85.4(4) . .
C1 Pt1 C3 88.3(3) . .
C2 Pt1 N1 90.4(3) . .
C1 Pt1 N1 178.3(3) . .
C3 Pt1 N1 91.0(3) . .
C2 Pt1 I2 178.1(3) . .
C1 Pt1 I2 90.8(2) . .
C3 Pt1 I2 93.0(3) . .
N1 Pt1 I2 90.76(14) . .
C2 Pt1 I1 94.7(3) . .
C1 Pt1 I1 90.1(2) . .
C3 Pt1 I1 178.4(2) . .
N1 Pt1 I1 90.65(15) . .
I2 Pt1 I1 86.804(16) . .
Pt1 I1 Pt1 92.00(2) . 6_556
Pt1 I2 Pt1 93.64(2) 6_556 .
C8 N1 C4 115.9(7) . .
C8 N1 Pt1 120.9(5) . .
C4 N1 Pt1 123.2(5) . .
Pt1 C1 H1A 109.5 . .
Pt1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Pt1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Pt1 C2 H2A 109.5 . .
Pt1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Pt1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Pt1 C3 H3A 109.5 . .
Pt1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Pt1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C4 C5 123.0(8) . .
N1 C4 H4 118.5 . .
C5 C4 H4 118.5 . .
C6 C5 C4 121.4(7) . .
C6 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
C5 C6 C7 116.3(7) . .
C5 C6 C9 123.9(7) . .
C7 C6 C9 119.8(7) . .
C8 C7 C6 119.3(7) . .
C8 C7 H7 120.4 . .
C6 C7 H7 120.4 . .
N1 C8 C7 124.1(7) . .
N1 C8 H8 117.9 . .
C7 C8 H8 117.9 . .
C6 C9 C10 111.0(6) . .
C6 C9 H9A 109.4 . .
C10 C9 H9A 109.4 . .
C6 C9 H9B 109.4 . .
C10 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C2 2.032(8) .
Pt1 C1 2.053(7) .
Pt1 C3 2.063(8) .
Pt1 N1 2.190(6) .
Pt1 I2 2.7784(5) .
Pt1 I1 2.8166(5) .
I1 Pt1 2.8166(5) 6_556
I2 Pt1 2.7784(5) 6_556
N1 C8 1.333(10) .
N1 C4 1.352(10) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.370(11) .
C4 H4 0.9500 .
C5 C6 1.365(11) .
C5 H5 0.9500 .
C6 C7 1.400(11) .
C6 C9 1.503(10) .
C7 C8 1.382(11) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C10 1.514(10) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C8 N1 C4 C5 1.6(11)
Pt1 N1 C4 C5 -176.7(6)
N1 C4 C5 C6 -1.3(12)
C4 C5 C6 C7 -0.2(11)
C4 C5 C6 C9 178.1(7)
C5 C6 C7 C8 1.1(10)
C9 C6 C7 C8 -177.2(7)
C4 N1 C8 C7 -0.6(10)
Pt1 N1 C8 C7 177.8(5)
C6 C7 C8 N1 -0.8(11)
C5 C6 C9 C10 -92.6(9)
C7 C6 C9 C10 85.6(9)
