#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:49:11 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180156 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/52/7105236.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_7105236
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_sum            'C33 H56 Cl2 N4 Pt'
_chemical_formula_weight         774.81
_chemical_name_common            (Pt(ICy)2Me2).(CH2Cl2)
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 105.3540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5185(7)
_cell_length_b                   12.9037(6)
_cell_length_c                   17.4636(8)
_cell_measurement_reflns_used    19806
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.533
_cell_measurement_theta_min      2.222
_cell_volume                     3372.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27974
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    4.347
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.720203
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         10221
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.1748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                8950
_reflns_number_total             10221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920482b.txt
_cod_data_source_block           nol189a
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7105236
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'
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 0.96832(3) 0.247626(7) 0.91242(2) 0.01112(2) Uani 1 1 d . . .
Cl1 Cl 1.08393(5) -0.02126(6) 1.05721(5) 0.03152(16) Uani 1 1 d . . .
N1 N 0.79042(14) 0.18101(16) 0.79200(12) 0.0141(4) Uani 1 1 d . . .
C1 C 0.8726(2) 0.2246(2) 0.80642(17) 0.0136(5) Uani 1 1 d . . .
Cl2 Cl 0.92782(7) -0.12528(8) 0.95691(6) 0.0501(2) Uani 1 1 d . . .
N2 N 0.87549(16) 0.26147(15) 0.73287(14) 0.0162(4) Uani 1 1 d . . .
C2 C 0.74271(18) 0.1901(2) 0.71269(16) 0.0195(5) Uani 1 1 d . . .
H2 H 0.6839 0.1656 0.6893 0.023 Uiso 1 1 calc R . .
N3 N 0.82814(13) 0.40117(16) 0.94248(12) 0.0136(4) Uani 1 1 d . . .
C3 C 0.7962(2) 0.24035(19) 0.67567(17) 0.0202(5) Uani 1 1 d . . .
H3 H 0.7824 0.2580 0.6210 0.024 Uiso 1 1 calc R . .
N4 N 0.86226(15) 0.28629(17) 1.03455(13) 0.0146(4) Uani 1 1 d . . .
C4 C 0.75327(17) 0.12943(19) 0.85176(15) 0.0151(5) Uani 1 1 d . . .
H4 H 0.7984 0.1334 0.9045 0.018 Uiso 1 1 calc R . .
C5 C 0.7345(2) 0.0150(2) 0.83010(18) 0.0228(6) Uani 1 1 d . . .
H5A H 0.6946 0.0097 0.7757 0.027 Uiso 1 1 calc R . .
H5B H 0.7913 -0.0205 0.8309 0.027 Uiso 1 1 calc R . .
C6 C 0.6909(2) -0.0381(2) 0.88838(19) 0.0263(6) Uani 1 1 d . . .
H6A H 0.6766 -0.1107 0.8713 0.032 Uiso 1 1 calc R . .
H6B H 0.7337 -0.0396 0.9416 0.032 Uiso 1 1 calc R . .
C7 C 0.6059(2) 0.0165(2) 0.89377(19) 0.0264(6) Uani 1 1 d . . .
H7A H 0.5602 0.0106 0.8422 0.032 Uiso 1 1 calc R . .
H7B H 0.5822 -0.0177 0.9347 0.032 Uiso 1 1 calc R . .
C8 C 0.62352(18) 0.1301(2) 0.91480(17) 0.0218(5) Uani 1 1 d . . .
H8A H 0.6623 0.1358 0.9697 0.026 Uiso 1 1 calc R . .
H8B H 0.5662 0.1651 0.9130 0.026 Uiso 1 1 calc R . .
C9 C 0.66846(18) 0.1848(2) 0.85796(17) 0.0199(5) Uani 1 1 d . . .
H9A H 0.6259 0.1884 0.8046 0.024 Uiso 1 1 calc R . .
H9B H 0.6836 0.2566 0.8766 0.024 Uiso 1 1 calc R . .
C10 C 0.95214(17) 0.31419(19) 0.71496(14) 0.0148(5) Uani 1 1 d . . .
H10 H 0.9949 0.3346 0.7664 0.018 Uiso 1 1 calc R . .
C11 C 0.92177(18) 0.4134(2) 0.66599(16) 0.0187(5) Uani 1 1 d . . .
H11A H 0.8776 0.3951 0.6156 0.022 Uiso 1 1 calc R . .
H11B H 0.8924 0.4606 0.6960 0.022 Uiso 1 1 calc R . .
C12 C 1.0011(2) 0.4686(2) 0.64772(17) 0.0228(6) Uani 1 1 d . . .
H12A H 0.9791 0.5286 0.6126 0.027 Uiso 1 1 calc R . .
H12B H 1.0410 0.4954 0.6978 0.027 Uiso 1 1 calc R . .
C13 C 1.05392(19) 0.3975(2) 0.60788(17) 0.0234(6) Uani 1 1 d . . .
H13A H 1.1078 0.4344 0.6020 0.028 Uiso 1 1 calc R . .
H13B H 1.0169 0.3793 0.5541 0.028 Uiso 1 1 calc R . .
C14 C 1.08221(19) 0.2984(2) 0.65590(17) 0.0223(6) Uani 1 1 d . . .
H14A H 1.1247 0.3159 0.7074 0.027 Uiso 1 1 calc R . .
H14B H 1.1130 0.2518 0.6267 0.027 Uiso 1 1 calc R . .
C15 C 1.0012(3) 0.2428(2) 0.6707(3) 0.0208(9) Uani 1 1 d . . .
H15A H 1.0210 0.1794 0.7025 0.025 Uiso 1 1 calc R . .
H15B H 0.9602 0.2218 0.6194 0.025 Uiso 1 1 calc R . .
C16 C 0.88167(17) 0.31594(19) 0.96605(15) 0.0129(5) Uani 1 1 d . . .
C17 C 0.77862(17) 0.4240(2) 0.99595(15) 0.0171(5) Uani 1 1 d . . .
H17 H 0.7379 0.4799 0.9926 0.020 Uiso 1 1 calc R . .
C18 C 0.79951(18) 0.3519(2) 1.05315(16) 0.0197(5) Uani 1 1 d . . .
H18 H 0.7759 0.3465 1.0979 0.024 Uiso 1 1 calc R . .
C19 C 0.82741(16) 0.46569(19) 0.87275(14) 0.0137(5) Uani 1 1 d . . .
H19 H 0.8635 0.4297 0.8410 0.016 Uiso 1 1 calc R . .
C20 C 0.73208(18) 0.4790(2) 0.82002(16) 0.0209(5) Uani 1 1 d . . .
H20A H 0.6934 0.5056 0.8525 0.025 Uiso 1 1 calc R . .
H20B H 0.7085 0.4107 0.7984 0.025 Uiso 1 1 calc R . .
C21 C 0.72849(18) 0.5541(2) 0.75105(16) 0.0215(6) Uani 1 1 d . . .
H21A H 0.7572 0.5211 0.7129 0.026 Uiso 1 1 calc R . .
H21B H 0.6653 0.5678 0.7229 0.026 Uiso 1 1 calc R . .
C22 C 0.77496(19) 0.6563(2) 0.77875(17) 0.0220(6) Uani 1 1 d . . .
H22A H 0.7757 0.6993 0.7320 0.026 Uiso 1 1 calc R . .
H22B H 0.7413 0.6943 0.8107 0.026 Uiso 1 1 calc R . .
C23 C 0.87009(18) 0.6383(2) 0.82830(16) 0.0207(5) Uani 1 1 d . . .
H23A H 0.8985 0.7058 0.8466 0.025 Uiso 1 1 calc R . .
H23B H 0.9049 0.6046 0.7953 0.025 Uiso 1 1 calc R . .
C24 C 0.87154(18) 0.5700(2) 0.90014(15) 0.0190(5) Uani 1 1 d . . .
H24A H 0.8392 0.6051 0.9347 0.023 Uiso 1 1 calc R . .
H24B H 0.9341 0.5588 0.9314 0.023 Uiso 1 1 calc R . .
C25 C 0.90292(17) 0.19725(18) 1.08533(15) 0.0141(5) Uani 1 1 d . . .
H25 H 0.9449 0.1618 1.0592 0.017 Uiso 1 1 calc R . .
C26 C 0.83166(19) 0.1194(2) 1.09170(16) 0.0204(5) Uani 1 1 d . . .
H26A H 0.8017 0.0927 1.0381 0.024 Uiso 1 1 calc R . .
H26B H 0.7860 0.1547 1.1127 0.024 Uiso 1 1 calc R . .
C27 C 0.8708(2) 0.0287(2) 1.14593(17) 0.0250(6) Uani 1 1 d . . .
H27A H 0.8219 -0.0174 1.1516 0.030 Uiso 1 1 calc R . .
H27B H 0.9109 -0.0120 1.1217 0.030 Uiso 1 1 calc R . .
C28 C 0.9228(2) 0.0669(2) 1.22721(17) 0.0272(6) Uani 1 1 d . . .
H28A H 0.9504 0.0071 1.2603 0.033 Uiso 1 1 calc R . .
H28B H 0.8815 0.1013 1.2537 0.033 Uiso 1 1 calc R . .
C29 C 0.9955(2) 0.1428(2) 1.22035(17) 0.0255(6) Uani 1 1 d . . .
H29A H 1.0401 0.1064 1.1988 0.031 Uiso 1 1 calc R . .
H29B H 1.0264 0.1691 1.2738 0.031 Uiso 1 1 calc R . .
C30 C 0.9567(3) 0.2341(2) 1.1663(3) 0.0197(8) Uani 1 1 d . . .
H30A H 0.9178 0.2756 1.1913 0.024 Uiso 1 1 calc R . .
H30B H 1.0059 0.2792 1.1600 0.024 Uiso 1 1 calc R . .
C31 C 1.0720(2) 0.2806(3) 1.01403(18) 0.0188(6) Uani 1 1 d . . .
H31A H 1.0558 0.3412 1.0411 0.028 Uiso 1 1 calc R . .
H31B H 1.1270 0.2952 0.9985 0.028 Uiso 1 1 calc R . .
H31C H 1.0815 0.2209 1.0499 0.028 Uiso 1 1 calc R . .
C32 C 1.06948(18) 0.1746(2) 0.87195(16) 0.0152(5) Uani 1 1 d . . .
H32A H 1.1019 0.2266 0.8496 0.023 Uiso 1 1 calc R . .
H32B H 1.0425 0.1236 0.8310 0.023 Uiso 1 1 calc R . .
H32C H 1.1111 0.1394 0.9165 0.023 Uiso 1 1 calc R . .
C33 C 1.0118(2) -0.0327(3) 0.95991(18) 0.0357(8) Uani 1 1 d . . .
H33A H 0.9839 0.0353 0.9426 0.043 Uiso 1 1 calc R . .
H33B H 1.0471 -0.0533 0.9227 0.043 Uiso 1 1 calc 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C16 Pt1 C1 93.96(11) . . ?
C16 Pt1 C31 88.56(12) . . ?
C1 Pt1 C31 174.40(14) . . ?
C16 Pt1 C32 172.45(11) . . ?
C1 Pt1 C32 93.30(11) . . ?
C31 Pt1 C32 84.39(12) . . ?
C1 N1 C2 112.1(2) . . ?
C1 N1 C4 125.4(2) . . ?
C2 N1 C4 122.5(2) . . ?
N1 C1 N2 103.3(2) . . ?
N1 C1 Pt1 130.1(2) . . ?
N2 C1 Pt1 126.2(2) . . ?
C1 N2 C3 111.1(2) . . ?
C1 N2 C10 125.6(2) . . ?
C3 N2 C10 123.2(2) . . ?
C3 C2 N1 106.6(2) . . ?
C16 N3 C17 111.5(2) . . ?
C16 N3 C19 124.9(2) . . ?
C17 N3 C19 123.5(2) . . ?
C2 C3 N2 106.9(2) . . ?
C16 N4 C18 111.4(2) . . ?
C16 N4 C25 125.7(2) . . ?
C18 N4 C25 122.9(2) . . ?
N1 C4 C9 110.1(2) . . ?
N1 C4 C5 110.1(2) . . ?
C9 C4 C5 110.9(2) . . ?
C6 C5 C4 110.9(2) . . ?
C7 C6 C5 112.2(2) . . ?
C8 C7 C6 111.0(2) . . ?
C7 C8 C9 111.9(2) . . ?
C4 C9 C8 112.4(2) . . ?
N2 C10 C15 111.5(2) . . ?
N2 C10 C11 110.8(2) . . ?
C15 C10 C11 109.9(2) . . ?
C12 C11 C10 111.0(2) . . ?
C13 C12 C11 112.1(2) . . ?
C12 C13 C14 111.5(2) . . ?
C13 C14 C15 110.9(2) . . ?
C14 C15 C10 110.1(2) . . ?
N4 C16 N3 103.3(2) . . ?
N4 C16 Pt1 127.56(18) . . ?
N3 C16 Pt1 129.09(19) . . ?
C18 C17 N3 106.6(2) . . ?
C17 C18 N4 107.1(2) . . ?
N3 C19 C24 109.5(2) . . ?
N3 C19 C20 110.8(2) . . ?
C24 C19 C20 111.8(2) . . ?
C19 C20 C21 111.8(2) . . ?
C22 C21 C20 112.5(2) . . ?
C23 C22 C21 110.9(2) . . ?
C22 C23 C24 110.9(2) . . ?
C23 C24 C19 110.1(2) . . ?
N4 C25 C30 110.9(2) . . ?
N4 C25 C26 110.6(2) . . ?
C30 C25 C26 111.7(2) . . ?
C25 C26 C27 112.0(2) . . ?
C28 C27 C26 110.9(2) . . ?
C27 C28 C29 110.9(2) . . ?
C28 C29 C30 111.4(3) . . ?
C25 C30 C29 111.3(2) . . ?
Cl2 C33 Cl1 111.06(17) . . ?
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 C16 2.032(3) . ?
Pt1 C1 2.065(3) . ?
Pt1 C31 2.099(3) . ?
Pt1 C32 2.107(3) . ?
Cl1 C33 1.776(3) . ?
N1 C1 1.355(4) . ?
N1 C2 1.392(3) . ?
N1 C4 1.477(3) . ?
C1 N2 1.382(4) . ?
Cl2 C33 1.758(4) . ?
N2 C3 1.391(4) . ?
N2 C10 1.474(3) . ?
C2 C3 1.346(4) . ?
N3 C16 1.374(3) . ?
N3 C17 1.389(3) . ?
N3 C19 1.473(3) . ?
N4 C16 1.363(3) . ?
N4 C18 1.392(3) . ?
N4 C25 1.486(3) . ?
C4 C9 1.526(4) . ?
C4 C5 1.532(4) . ?
C5 C6 1.527(4) . ?
C6 C7 1.520(4) . ?
C7 C8 1.519(4) . ?
C8 C9 1.528(4) . ?
C10 C15 1.529(5) . ?
C10 C11 1.542(4) . ?
C11 C12 1.528(4) . ?
C12 C13 1.516(4) . ?
C13 C14 1.529(4) . ?
C14 C15 1.528(5) . ?
C17 C18 1.341(4) . ?
C19 C24 1.529(4) . ?
C19 C20 1.531(4) . ?
C20 C21 1.535(4) . ?
C21 C22 1.519(4) . ?
C22 C23 1.518(4) . ?
C23 C24 1.529(3) . ?
C25 C30 1.516(5) . ?
C25 C26 1.519(4) . ?
C26 C27 1.528(4) . ?
C27 C28 1.518(4) . ?
C28 C29 1.522(4) . ?
C29 C30 1.530(4) . ?
