#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:49:11 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180156 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/52/7105235.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_7105235
loop_
_publ_author_name
'Fortman, George C'
'Scott, Natalie M'
'Linden, Anthony'
'Stevens, Edwin D'
'Dorta, Reto'
'Nolan, Steven P'
_publ_section_title
;
 Unusual reactivities of N-heterocyclic carbenes upon coordination to
 the platinum(II)-dimethyl moiety.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1050
_journal_page_last               1052
_journal_paper_doi               10.1039/b920482b
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C16 H30 N4 Pt'
_chemical_formula_sum            'C16 H30 N4 Pt'
_chemical_formula_weight         473.44
_chemical_name_common            (MeIMe)2Pt(Me)2
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             07-03-06
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5403(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8926(2)
_cell_length_b                   8.1788(1)
_cell_length_c                   16.1119(2)
_cell_measurement_reflns_used    34346
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     1799.17(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 '65 mm CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scans with κ offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50417
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.765
_exptl_absorpt_correction_T_max  0.390
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.161
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0375
_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)+(0.0573P)²+5.7916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                4641
_reflns_number_total             5253
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            b920482b.txt
_cod_data_source_block           DT0707
_cod_database_code               7105235
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.180706(11) 0.209733(19) 0.436874(10) 0.01729(7) Uani 1 1 d . . .
N2 N 0.3746(3) 0.0309(5) 0.5420(2) 0.0207(7) Uani 1 1 d . . .
N5 N 0.2766(3) -0.1190(5) 0.4357(3) 0.0228(7) Uani 1 1 d . . .
N11 N 0.1280(3) 0.0504(5) 0.5841(2) 0.0193(7) Uani 1 1 d . . .
N14 N 0.1635(3) 0.3031(4) 0.6149(3) 0.0189(7) Uani 1 1 d . . .
C1 C 0.2826(3) 0.0319(6) 0.4730(3) 0.0198(8) Uani 1 1 d . . .
C3 C 0.4226(3) -0.1169(7) 0.5469(3) 0.0256(9) Uani 1 1 d . . .
C4 C 0.3601(4) -0.2124(6) 0.4797(4) 0.0269(10) Uani 1 1 d . . .
C6 C 0.4153(4) 0.1708(7) 0.5982(4) 0.0284(10) Uani 1 1 d . . .
H61 H 0.4743 0.2067 0.5906 0.043 Uiso 1 1 calc R . .
H62 H 0.4322 0.1417 0.6617 0.043 Uiso 1 1 calc R . .
H63 H 0.3670 0.2596 0.5807 0.043 Uiso 1 1 calc R . .
C7 C 0.5240(4) -0.1485(8) 0.6143(4) 0.0374(13) Uani 1 1 d . . .
H71 H 0.5402 -0.2641 0.6120 0.056 Uiso 1 1 calc R . .
H72 H 0.5284 -0.1218 0.6751 0.056 Uiso 1 1 calc R . .
H73 H 0.5702 -0.0805 0.6001 0.056 Uiso 1 1 calc R . .
C8 C 0.3679(5) -0.3854(7) 0.4527(4) 0.0386(13) Uani 1 1 d . . .
H81 H 0.4301 -0.4324 0.4944 0.058 Uiso 1 1 calc R . .
H82 H 0.3652 -0.3873 0.3909 0.058 Uiso 1 1 calc R . .
H83 H 0.3135 -0.4497 0.4551 0.058 Uiso 1 1 calc R . .
C9 C 0.1913(4) -0.1742(7) 0.3568(4) 0.0306(11) Uani 1 1 d . . .
H91 H 0.1433 -0.0855 0.3356 0.046 Uiso 1 1 calc R . .
H92 H 0.1617 -0.2686 0.3737 0.046 Uiso 1 1 calc R . .
H93 H 0.2119 -0.2057 0.3084 0.046 Uiso 1 1 calc R . .
C10 C 0.1574(3) 0.1851(5) 0.5519(3) 0.0179(8) Uani 1 1 d . . .
C12 C 0.1158(3) 0.0821(6) 0.6643(3) 0.0212(8) Uani 1 1 d . . .
C13 C 0.1380(3) 0.2419(6) 0.6828(3) 0.0204(8) Uani 1 1 d . . .
C15 C 0.1108(4) -0.1076(6) 0.5393(3) 0.0257(9) Uani 1 1 d . . .
H151 H 0.0973 -0.0924 0.4751 0.039 Uiso 1 1 calc R . .
H152 H 0.0546 -0.1605 0.5451 0.039 Uiso 1 1 calc R . .
H153 H 0.1690 -0.1764 0.5675 0.039 Uiso 1 1 calc R . .
C16 C 0.0796(4) -0.0433(8) 0.7098(4) 0.0344(12) Uani 1 1 d . . .
H161 H 0.0788 0.0023 0.7658 0.052 Uiso 1 1 calc R . .
H162 H 0.1229 -0.1387 0.7242 0.052 Uiso 1 1 calc R . .
H163 H 0.0131 -0.0762 0.6696 0.052 Uiso 1 1 calc R . .
C17 C 0.1379(4) 0.3450(8) 0.7592(3) 0.0314(11) Uani 1 1 d . . .
H171 H 0.0864 0.4280 0.7359 0.047 Uiso 1 1 calc R . .
H172 H 0.2017 0.3989 0.7887 0.047 Uiso 1 1 calc R . .
H173 H 0.1256 0.2759 0.8032 0.047 Uiso 1 1 calc R . .
C18 C 0.1867(4) 0.4729(6) 0.6070(3) 0.0266(9) Uani 1 1 d . . .
H181 H 0.1266 0.5384 0.5874 0.040 Uiso 1 1 calc R . .
H182 H 0.2157 0.4827 0.5623 0.040 Uiso 1 1 calc R . .
H183 H 0.2333 0.5125 0.6658 0.040 Uiso 1 1 calc R . .
C19 C 0.1968(5) 0.2425(8) 0.3149(4) 0.0346(12) Uani 1 1 d . . .
H191 H 0.2459 0.1657 0.3118 0.052 Uiso 1 1 calc R . .
H192 H 0.2181 0.3547 0.3115 0.052 Uiso 1 1 calc R . .
H193 H 0.1339 0.2223 0.2641 0.052 Uiso 1 1 calc R . .
C20 C 0.0728(3) 0.3950(6) 0.3892(3) 0.0255(9) Uani 1 1 d . . .
H201 H 0.1038 0.4983 0.3845 0.038 Uiso 1 1 calc R . .
H202 H 0.0410 0.4080 0.4316 0.038 Uiso 1 1 calc R . .
H203 H 0.0238 0.3644 0.3295 0.038 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 64 0.0033 0.0016
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
H H 120 0.0000 0.0000
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
N N 16 0.0061 0.0033
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
Pt Pt 4 -1.7033 8.3905
; International Tables for Crystallography (1992).
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
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
_geom_angle_publ_flag
C1 Pt1 C10 92.78(17) . . ?
C1 Pt1 C19 90.5(2) . . ?
C10 Pt1 C19 176.6(2) . . ?
C1 Pt1 C20 175.87(18) . . ?
C10 Pt1 C20 91.17(18) . . ?
C19 Pt1 C20 85.6(2) . . ?
C1 N2 C3 112.0(4) . . ?
C1 N2 C6 122.5(4) . . ?
C3 N2 C6 125.4(4) . . ?
C1 N5 C4 112.7(4) . . ?
C1 N5 C9 123.0(4) . . ?
C4 N5 C9 124.2(4) . . ?
C10 N11 C12 112.4(4) . . ?
C10 N11 C15 123.4(4) . . ?
C12 N11 C15 124.2(4) . . ?
C10 N14 C13 111.7(4) . . ?
C10 N14 C18 123.7(4) . . ?
C13 N14 C18 124.4(4) . . ?
N5 C1 N2 102.7(4) . . ?
N5 C1 Pt1 128.2(3) . . ?
N2 C1 Pt1 129.0(3) . . ?
C4 C3 N2 106.3(4) . . ?
C4 C3 C7 130.9(5) . . ?
N2 C3 C7 122.8(5) . . ?
C3 C4 N5 106.2(4) . . ?
C3 C4 C8 131.8(5) . . ?
N5 C4 C8 122.0(5) . . ?
N2 C6 H61 109.5 . . ?
N2 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
N2 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
C3 C7 H71 109.5 . . ?
C3 C7 H72 109.5 . . ?
H71 C7 H72 109.5 . . ?
C3 C7 H73 109.5 . . ?
H71 C7 H73 109.5 . . ?
H72 C7 H73 109.5 . . ?
C4 C8 H81 109.5 . . ?
C4 C8 H82 109.5 . . ?
H81 C8 H82 109.5 . . ?
C4 C8 H83 109.5 . . ?
H81 C8 H83 109.5 . . ?
H82 C8 H83 109.5 . . ?
N5 C9 H91 109.5 . . ?
N5 C9 H92 109.5 . . ?
H91 C9 H92 109.5 . . ?
N5 C9 H93 109.5 . . ?
H91 C9 H93 109.5 . . ?
H92 C9 H93 109.5 . . ?
N11 C10 N14 102.9(4) . . ?
N11 C10 Pt1 128.8(3) . . ?
N14 C10 Pt1 128.3(3) . . ?
C13 C12 N11 105.8(4) . . ?
C13 C12 C16 131.7(5) . . ?
N11 C12 C16 122.4(5) . . ?
C12 C13 N14 107.2(4) . . ?
C12 C13 C17 130.3(5) . . ?
N14 C13 C17 122.5(4) . . ?
N11 C15 H151 109.5 . . ?
N11 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
N11 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
C12 C16 H161 109.5 . . ?
C12 C16 H162 109.5 . . ?
H161 C16 H162 109.5 . . ?
C12 C16 H163 109.5 . . ?
H161 C16 H163 109.5 . . ?
H162 C16 H163 109.5 . . ?
C13 C17 H171 109.5 . . ?
C13 C17 H172 109.5 . . ?
H171 C17 H172 109.5 . . ?
C13 C17 H173 109.5 . . ?
H171 C17 H173 109.5 . . ?
H172 C17 H173 109.5 . . ?
N14 C18 H181 109.5 . . ?
N14 C18 H182 109.5 . . ?
H181 C18 H182 109.5 . . ?
N14 C18 H183 109.5 . . ?
H181 C18 H183 109.5 . . ?
H182 C18 H183 109.5 . . ?
Pt1 C19 H191 109.5 . . ?
Pt1 C19 H192 109.5 . . ?
H191 C19 H192 109.5 . . ?
Pt1 C19 H193 109.5 . . ?
H191 C19 H193 109.5 . . ?
H192 C19 H193 109.5 . . ?
Pt1 C20 H201 109.5 . . ?
Pt1 C20 H202 109.5 . . ?
H201 C20 H202 109.5 . . ?
Pt1 C20 H203 109.5 . . ?
H201 C20 H203 109.5 . . ?
H202 C20 H203 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C1 2.013(4) . ?
Pt1 C10 2.027(5) . ?
Pt1 C19 2.090(6) . ?
Pt1 C20 2.117(5) . ?
N2 C1 1.377(5) . ?
N2 C3 1.390(6) . ?
N2 C6 1.435(6) . ?
N5 C1 1.360(6) . ?
N5 C4 1.388(6) . ?
N5 C9 1.464(6) . ?
N11 C10 1.363(6) . ?
N11 C12 1.399(6) . ?
N11 C15 1.451(6) . ?
N14 C10 1.376(6) . ?
N14 C13 1.387(6) . ?
N14 C18 1.449(6) . ?
C3 C4 1.359(8) . ?
C3 C7 1.488(7) . ?
C4 C8 1.498(7) . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
C7 H71 0.9800 . ?
C7 H72 0.9800 . ?
C7 H73 0.9800 . ?
C8 H81 0.9800 . ?
C8 H82 0.9800 . ?
C8 H83 0.9800 . ?
C9 H91 0.9800 . ?
C9 H92 0.9800 . ?
C9 H93 0.9800 . ?
C12 C13 1.352(7) . ?
C12 C16 1.482(6) . ?
C13 C17 1.493(7) . ?
C15 H151 0.9800 . ?
C15 H152 0.9800 . ?
C15 H153 0.9800 . ?
C16 H161 0.9800 . ?
C16 H162 0.9800 . ?
C16 H163 0.9800 . ?
C17 H171 0.9800 . ?
C17 H172 0.9800 . ?
C17 H173 0.9800 . ?
C18 H181 0.9800 . ?
C18 H182 0.9800 . ?
C18 H183 0.9800 . ?
C19 H191 0.9800 . ?
C19 H192 0.9800 . ?
C19 H193 0.9800 . ?
C20 H201 0.9800 . ?
C20 H202 0.9800 . ?
C20 H203 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N5 C1 N2 0.9(5) . . . . ?
C9 N5 C1 N2 -178.3(4) . . . . ?
C4 N5 C1 Pt1 -178.1(3) . . . . ?
C9 N5 C1 Pt1 2.6(6) . . . . ?
C3 N2 C1 N5 -0.6(5) . . . . ?
C6 N2 C1 N5 176.9(4) . . . . ?
C3 N2 C1 Pt1 178.5(3) . . . . ?
C6 N2 C1 Pt1 -4.0(6) . . . . ?
C10 Pt1 C1 N5 110.8(4) . . . . ?
C19 Pt1 C1 N5 -68.1(4) . . . . ?
C10 Pt1 C1 N2 -68.0(4) . . . . ?
C19 Pt1 C1 N2 113.0(4) . . . . ?
C1 N2 C3 C4 0.0(5) . . . . ?
C6 N2 C3 C4 -177.4(4) . . . . ?
C1 N2 C3 C7 178.6(4) . . . . ?
C6 N2 C3 C7 1.2(7) . . . . ?
N2 C3 C4 N5 0.5(5) . . . . ?
C7 C3 C4 N5 -177.9(5) . . . . ?
N2 C3 C4 C8 -177.4(5) . . . . ?
C7 C3 C4 C8 4.2(10) . . . . ?
C1 N5 C4 C3 -0.9(6) . . . . ?
C9 N5 C4 C3 178.3(4) . . . . ?
C1 N5 C4 C8 177.2(5) . . . . ?
C9 N5 C4 C8 -3.6(8) . . . . ?
C12 N11 C10 N14 0.1(5) . . . . ?
C15 N11 C10 N14 179.8(4) . . . . ?
C12 N11 C10 Pt1 -177.4(3) . . . . ?
C15 N11 C10 Pt1 2.2(6) . . . . ?
C13 N14 C10 N11 -0.4(5) . . . . ?
C18 N14 C10 N11 -176.0(4) . . . . ?
C13 N14 C10 Pt1 177.2(3) . . . . ?
C18 N14 C10 Pt1 1.5(6) . . . . ?
C1 Pt1 C10 N11 -58.7(4) . . . . ?
C20 Pt1 C10 N11 120.1(4) . . . . ?
C1 Pt1 C10 N14 124.4(4) . . . . ?
C20 Pt1 C10 N14 -56.8(4) . . . . ?
C10 N11 C12 C13 0.1(5) . . . . ?
C15 N11 C12 C13 -179.5(4) . . . . ?
C10 N11 C12 C16 177.0(4) . . . . ?
C15 N11 C12 C16 -2.6(7) . . . . ?
N11 C12 C13 N14 -0.4(5) . . . . ?
C16 C12 C13 N14 -176.8(5) . . . . ?
N11 C12 C13 C17 179.7(5) . . . . ?
C16 C12 C13 C17 3.3(9) . . . . ?
C10 N14 C13 C12 0.5(5) . . . . ?
C18 N14 C13 C12 176.1(4) . . . . ?
C10 N14 C13 C17 -179.6(4) . . . . ?
C18 N14 C13 C17 -4.0(7) . . . . ?
