#------------------------------------------------------------------------------
#$Date: 2019-10-16 04:16:26 +0300 (Wed, 16 Oct 2019) $
#$Revision: 219379 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/13/7701380.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_7701380
loop_
_publ_author_name
'Rehm, Tobias'
'Rothemund, Matthias'
'Dietel, Thomas'
'Kempe, Rhett'
'Schobert, Rainer'
_publ_section_title
;
 Synthesis, structures and cytotoxic effects in vitro of cis- and
 trans-[PtIVCl4(NHC)2] complexes and their PtII precursors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02438G
_journal_year                    2019
_chemical_formula_moiety         'C34 H32 Cl4 N4 Pt0.90, 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H36 Cl8 N4 Pt0.9'
_chemical_formula_weight         983.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 121.662(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   24.684(5)
_cell_length_b                   8.277(5)
_cell_length_c                   22.505(5)
_cell_measurement_reflns_used    8743
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      1.94
_cell_volume                     3914(3)
_computing_cell_refinement       STOE-XAREA
_computing_data_collection       STOE-XAREA
_computing_data_reduction        STOE-XAREA
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  STOE-STADIVARI
_diffrn_measurement_method       omega-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10695
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.988
_exptl_absorpt_coefficient_mu    3.808
_exptl_absorpt_correction_T_max  0.9116
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   STOE-XRED32
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             1945
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.139
_refine_diff_density_min         -2.777
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3414
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1072P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2307
_reflns_number_total             3414
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02438g2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C36 H36 Cl8 N4 Pt0.90'
_cod_database_code               7701380
_shelx_shelxl_version_number     2016/4
_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.
;
loop_
_space_group_symop_operation_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.6460(5) -0.0755(13) 0.7011(5) 0.047(3) Uani 1 1 d . . .
H1 H 0.637293 0.036785 0.698979 0.056 Uiso 1 1 calc R U .
C2 C 0.6878(5) -0.1285(14) 0.6835(7) 0.055(3) Uani 1 1 d . . .
H2 H 0.708358 -0.052464 0.670137 0.066 Uiso 1 1 calc R U .
C3 C 0.7011(5) -0.2904(16) 0.6846(6) 0.059(3) Uani 1 1 d . . .
H3 H 0.729756 -0.326815 0.671397 0.070 Uiso 1 1 calc R U .
C4 C 0.6717(5) -0.3984(15) 0.7054(6) 0.055(3) Uani 1 1 d . . .
H4 H 0.680481 -0.510594 0.706949 0.066 Uiso 1 1 calc R U .
C5 C 0.6296(5) -0.3443(13) 0.7240(5) 0.048(3) Uani 1 1 d . . .
H5 H 0.609937 -0.420223 0.738482 0.057 Uiso 1 1 calc R U .
C6 C 0.6157(4) -0.1821(12) 0.7220(5) 0.035(2) Uani 1 1 d . . .
C7 C 0.5690(4) -0.1276(12) 0.7426(5) 0.038(2) Uani 1 1 d . . .
H7A H 0.558066 -0.220415 0.762116 0.046 Uiso 1 1 calc R U .
H7B H 0.589149 -0.043669 0.779245 0.046 Uiso 1 1 calc R U .
C8 C 0.4760(4) 0.0704(11) 0.6758(4) 0.031(2) Uani 1 1 d . . .
C9 C 0.4789(4) -0.1472(12) 0.6199(5) 0.038(2) Uani 1 1 d . . .
H9 H 0.492929 -0.244956 0.610145 0.045 Uiso 1 1 calc R U .
C10 C 0.4258(4) -0.0690(12) 0.5767(5) 0.038(2) Uani 1 1 d . . .
H10 H 0.394890 -0.099761 0.530214 0.045 Uiso 1 1 calc R U .
C11 C 0.3690(4) 0.1802(12) 0.5758(5) 0.037(2) Uani 1 1 d . . .
H11A H 0.373059 0.246098 0.541640 0.044 Uiso 1 1 calc R U .
H11B H 0.369338 0.254159 0.610580 0.044 Uiso 1 1 calc R U .
C12 C 0.3068(4) 0.0881(12) 0.5386(5) 0.041(2) Uani 1 1 d . . .
C13 C 0.2821(5) 0.0206(14) 0.5760(6) 0.052(3) Uani 1 1 d . . .
H13 H 0.304557 0.030855 0.625363 0.063 Uiso 1 1 calc R U .
C14 C 0.2248(5) -0.0616(15) 0.5413(8) 0.067(4) Uani 1 1 d . . .
H14 H 0.207812 -0.106141 0.567064 0.080 Uiso 1 1 calc R U .
C15 C 0.1922(6) -0.0795(14) 0.4701(8) 0.076(4) Uani 1 1 d . . .
H15 H 0.152909 -0.136112 0.446869 0.091 Uiso 1 1 calc R U .
C16 C 0.2167(5) -0.0148(14) 0.4320(6) 0.060(3) Uani 1 1 d . . .
H16 H 0.194724 -0.027970 0.382771 0.072 Uiso 1 1 calc R U .
C17 C 0.2740(5) 0.0695(14) 0.4671(5) 0.051(3) Uani 1 1 d . . .
H17 H 0.290846 0.115052 0.441318 0.062 Uiso 1 1 calc R U .
C18 C 0.4756(7) -0.2389(19) 0.4329(8) 0.083(5) Uani 1 1 d . . .
H18A H 0.480760 -0.314303 0.402057 0.099 Uiso 1 1 calc R U .
H18B H 0.470365 -0.128673 0.413493 0.099 Uiso 1 1 calc R U .
N1 N 0.4237(3) 0.0663(9) 0.6115(4) 0.0328(17) Uani 1 1 d . . .
N2 N 0.5102(3) -0.0619(9) 0.6817(4) 0.0336(17) Uani 1 1 d . . .
CL1 Cl 0.47063(11) 0.4548(3) 0.66605(13) 0.0409(6) Uani 1 1 d . U .
CL2 Cl 0.40020(10) 0.2574(3) 0.73743(11) 0.0368(5) Uani 1 1 d . U .
CL3 Cl 0.4058(2) -0.2922(6) 0.4333(2) 0.0984(15) Uani 1 1 d . . .
CL4 Cl 0.5439(2) -0.2449(5) 0.5164(2) 0.0897(13) Uani 1 1 d . . .
PT1 Pt 0.500000 0.24545(6) 0.750000 0.0249(2) Uani 0.9 2 d S TU P
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
C2 C1 C6 121.4(11) . .
C1 C2 C3 121.2(11) . .
C2 C3 C4 118.5(11) . .
C3 C4 C5 120.4(11) . .
C6 C5 C4 121.2(11) . .
C5 C6 C1 117.4(9) . .
C5 C6 C7 119.6(9) . .
C1 C6 C7 123.0(9) . .
N2 C7 C6 111.0(7) . .
N1 C8 N2 106.5(8) . .
N1 C8 PT1 126.8(6) . .
N2 C8 PT1 126.7(6) . .
C10 C9 N2 107.8(9) . .
C9 C10 N1 107.3(8) . .
N1 C11 C12 110.4(8) . .
C17 C12 C13 119.2(10) . .
C17 C12 C11 120.3(10) . .
C13 C12 C11 120.5(9) . .
C14 C13 C12 120.0(11) . .
C15 C14 C13 120.7(13) . .
C14 C15 C16 120.1(12) . .
C15 C16 C17 119.0(11) . .
C12 C17 C16 121.1(12) . .
CL4 C18 CL3 112.2(8) . .
C8 N1 C10 109.3(7) . .
C8 N1 C11 130.8(8) . .
C10 N1 C11 120.0(7) . .
C8 N2 C9 109.1(7) . .
C8 N2 C7 130.5(8) . .
C9 N2 C7 120.2(8) . .
C8 PT1 C8 90.0(5) 2_656 .
C8 PT1 CL2 95.5(2) 2_656 2_656
C8 PT1 CL2 87.9(2) . 2_656
C8 PT1 CL2 87.9(2) 2_656 .
C8 PT1 CL2 95.5(2) . .
CL2 PT1 CL2 175.12(11) 2_656 .
C8 PT1 CL1 177.8(2) 2_656 .
C8 PT1 CL1 91.7(3) . .
CL2 PT1 CL1 85.83(8) 2_656 .
CL2 PT1 CL1 90.61(8) . .
C8 PT1 CL1 91.7(3) 2_656 2_656
C8 PT1 CL1 177.8(2) . 2_656
CL2 PT1 CL1 90.61(8) 2_656 2_656
CL2 PT1 CL1 85.83(8) . 2_656
CL1 PT1 CL1 86.50(13) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.358(14) .
C1 C6 1.389(14) .
C2 C3 1.376(17) .
C3 C4 1.377(17) .
C4 C5 1.383(15) .
C5 C6 1.381(15) .
C6 C7 1.519(13) .
C7 N2 1.482(11) .
C8 N1 1.342(11) .
C8 N2 1.345(11) .
C8 PT1 2.050(9) .
C9 C10 1.320(13) .
C9 N2 1.379(12) .
C10 N1 1.384(11) .
C11 N1 1.490(11) .
C11 C12 1.513(13) .
C12 C17 1.378(14) .
C12 C13 1.390(14) .
C13 C14 1.383(15) .
C14 C15 1.372(19) .
C15 C16 1.391(19) .
C16 C17 1.392(15) .
C18 CL4 1.747(16) .
C18 CL3 1.782(14) .
CL1 PT1 2.379(2) .
CL2 PT1 2.330(2) .
PT1 C8 2.050(9) 2_656
PT1 CL2 2.329(2) 2_656
PT1 CL1 2.379(2) 2_656
