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#$Date: 2019-11-23 04:47:51 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232160 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/70/4347080.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_4347080
loop_
_publ_author_name
'Sivchik, Vasily V.'
'Grachova, Elena V.'
'Melnikov, Alexei S.'
'Smirnov, Sergey N.'
'Ivanov, Alexander Yu'
'Hirva, Pipsa'
'Tunik, Sergey P.'
'Koshevoy, Igor O.'
_publ_section_title
;
 Solid-State and Solution Metallophilic Aggregation of a Cationic
 [Pt(NCN)L](+) Cyclometalated Complex.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3351
_journal_page_last               3363
_journal_paper_doi               10.1021/acs.inorgchem.5b02713
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '4(C18 H14 N3 Pt), 4(Cl O4), C2 H3 N'
_chemical_formula_sum            'C74 H59 Cl4 N13 O16 Pt4'
_chemical_formula_weight         2308.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.186(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.9845(6)
_cell_length_b                   21.5813(10)
_cell_length_c                   6.6105(3)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.92
_cell_measurement_theta_min      2.48
_cell_volume                     1810.67(14)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.4.01 (Brandenburg, 2014)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '62mm x 62mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            17806
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         1.861
_exptl_absorpt_coefficient_mu    7.929
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_description       needle
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.717
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3936
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0109P)²+1.6014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3438
_reflns_number_total             3936
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02713_si_002.cif
_cod_data_source_block           2ClO4120
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347080
_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   0.177
_shelx_estimated_absorpt_t_max   0.712
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.3214(2) 0.17610(14) 0.3532(4) 0.0198(6) Uani 1 1 d . . .
C2 C 0.4286(3) 0.16575(14) 0.3817(5) 0.0226(6) Uani 1 1 d . . .
C3 C 0.4652(3) 0.10456(15) 0.3898(5) 0.0287(7) Uani 1 1 d . . .
H15 H 0.5384 0.0961 0.4083 0.034 Uiso 1 1 calc R U .
C4 C 0.3930(3) 0.05671(16) 0.3704(6) 0.0327(8) Uani 1 1 d . . .
H14 H 0.4179 0.0152 0.3768 0.039 Uiso 1 1 calc R U .
C5 C 0.2844(3) 0.06718(15) 0.3417(5) 0.0294(7) Uani 1 1 d . . .
H13 H 0.2365 0.0334 0.3288 0.035 Uiso 1 1 calc R U .
C6 C 0.2479(3) 0.12785(14) 0.3325(5) 0.0228(7) Uani 1 1 d . . .
C7 C 0.4736(3) 0.33202(15) 0.3964(5) 0.0266(7) Uani 1 1 d . . .
H1 H 0.4307 0.3680 0.3888 0.032 Uiso 1 1 calc R U .
C8 C 0.5812(3) 0.33895(16) 0.4201(5) 0.0291(7) Uani 1 1 d . . .
H2 H 0.6119 0.3791 0.4283 0.035 Uiso 1 1 calc R U .
C9 C 0.6436(3) 0.28673(17) 0.4317(5) 0.0304(7) Uani 1 1 d . . .
H3 H 0.7177 0.2906 0.4470 0.036 Uiso 1 1 calc R U .
C10 C 0.5976(3) 0.22879(16) 0.4208(5) 0.0266(7) Uani 1 1 d . . .
H4 H 0.6400 0.1926 0.4291 0.032 Uiso 1 1 calc R U .
C11 C 0.4895(2) 0.22355(14) 0.3979(4) 0.0220(6) Uani 1 1 d . . .
C12 C 0.0344(2) 0.23919(15) 0.2782(5) 0.0233(6) Uani 1 1 d . . .
H100 H 0.0289 0.2831 0.2788 0.028 Uiso 1 1 calc R U .
C13 C -0.0566(3) 0.20424(15) 0.2539(5) 0.0270(7) Uani 1 1 d . . .
H10 H -0.1233 0.2238 0.2395 0.032 Uiso 1 1 calc R U .
C14 C -0.0491(3) 0.14053(16) 0.2510(5) 0.0309(8) Uani 1 1 d . . .
H11 H -0.1107 0.1156 0.2325 0.037 Uiso 1 1 calc R U .
C15 C 0.0497(3) 0.11316(15) 0.2753(5) 0.0264(7) Uani 1 1 d . . .
H12 H 0.0560 0.0693 0.2742 0.032 Uiso 1 1 calc R U .
C16 C 0.1389(3) 0.15015(13) 0.3011(5) 0.0217(6) Uani 1 1 d . . .
C17 C 0.1881(3) 0.40153(15) 0.3121(5) 0.0250(7) Uani 1 1 d . . .
C18 C 0.1542(3) 0.46594(16) 0.2972(6) 0.0404(9) Uani 1 1 d . . .
H17A H 0.0771 0.4677 0.2726 0.061 Uiso 1 1 calc R U .
H17B H 0.1781 0.4860 0.1823 0.061 Uiso 1 1 calc R U .
H17C H 0.1844 0.4874 0.4267 0.061 Uiso 1 1 calc R U .
C19 C 0.397(2) 0.494(5) 0.379(10) 0.048(2) Uani 0.25 1 d D . P
H19A H 0.3669 0.5352 0.3427 0.072 Uiso 0.25 1 calc R U P
H19B H 0.3527 0.4718 0.4589 0.072 Uiso 0.25 1 calc R U P
H19C H 0.3988 0.4708 0.2528 0.072 Uiso 0.25 1 calc R U P
C20 C 0.5000 0.5000 0.5000 0.047(3) Uani 0.5 2 d DS . P
N1 N 0.4276(2) 0.27588(11) 0.3836(4) 0.0204(5) Uani 1 1 d . . .
N2 N 0.1298(2) 0.21345(11) 0.3009(4) 0.0205(5) Uani 1 1 d . . .
N3 N 0.2150(2) 0.35123(12) 0.3232(4) 0.0228(6) Uani 1 1 d . . .
N4 N 0.4154(17) 0.495(4) 0.398(8) 0.048(2) Uani 0.25 1 d D . P
O2 O 0.7731(2) 0.42217(11) 0.3438(5) 0.0451(7) Uani 1 1 d . . .
O3 O 0.7440(2) 0.41060(14) -0.0141(5) 0.0523(7) Uani 1 1 d . . .
O4 O 0.8542(2) 0.34180(12) 0.2001(5) 0.0511(8) Uani 1 1 d . . .
O5 O 0.9057(2) 0.44477(13) 0.1658(5) 0.0533(8) Uani 1 1 d . . .
Cl1 Cl 0.81947(6) 0.40412(3) 0.17449(13) 0.02707(17) Uani 1 1 d . . .
Pt1 Pt 0.27013(2) 0.25932(2) 0.34077(2) 0.01788(4) Uani 1 1 d . . .
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'
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 122.6(3) . .
C2 C1 Pt1 119.3(2) . .
C6 C1 Pt1 118.1(2) . .
C1 C2 C3 118.7(3) . .
C1 C2 C11 112.6(3) . .
C3 C2 C11 128.7(3) . .
C4 C3 C2 118.9(3) . .
C4 C3 H15 120.6 . .
C2 C3 H15 120.6 . .
C3 C4 C5 122.4(3) . .
C3 C4 H14 118.8 . .
C5 C4 H14 118.8 . .
C6 C5 C4 118.8(3) . .
C6 C5 H13 120.6 . .
C4 C5 H13 120.6 . .
C5 C6 C1 118.5(3) . .
C5 C6 C16 128.7(3) . .
C1 C6 C16 112.8(3) . .
N1 C7 C8 122.0(3) . .
N1 C7 H1 119.0 . .
C8 C7 H1 119.0 . .
C9 C8 C7 119.1(3) . .
C9 C8 H2 120.5 . .
C7 C8 H2 120.5 . .
C8 C9 C10 119.6(3) . .
C8 C9 H3 120.2 . .
C10 C9 H3 120.2 . .
C9 C10 C11 119.8(3) . .
C9 C10 H4 120.1 . .
C11 C10 H4 120.1 . .
N1 C11 C10 120.3(3) . .
N1 C11 C2 113.2(3) . .
C10 C11 C2 126.5(3) . .
N2 C12 C13 122.4(3) . .
N2 C12 H100 118.8 . .
C13 C12 H100 118.8 . .
C14 C13 C12 119.0(3) . .
C14 C13 H10 120.5 . .
C12 C13 H10 120.5 . .
C13 C14 C15 119.2(3) . .
C13 C14 H11 120.4 . .
C15 C14 H11 120.4 . .
C16 C15 C14 119.7(3) . .
C16 C15 H12 120.1 . .
C14 C15 H12 120.1 . .
N2 C16 C15 120.2(3) . .
N2 C16 C6 114.0(3) . .
C15 C16 C6 125.7(3) . .
N3 C17 C18 179.7(4) . .
C17 C18 H17A 109.5 . .
C17 C18 H17B 109.5 . .
H17A C18 H17B 109.5 . .
C17 C18 H17C 109.5 . .
H17A C18 H17C 109.5 . .
H17B C18 H17C 109.5 . .
C20 C19 H19A 109.5 . .
C20 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C20 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N4 C20 N4 179.998(14) . 3_666
N4 C20 C19 1(6) . .
N4 C20 C19 179(6) 3_666 .
N4 C20 C19 179(6) . 3_666
N4 C20 C19 1(6) 3_666 3_666
C19 C20 C19 179.997(13) . 3_666
C7 N1 C11 119.3(3) . .
C7 N1 Pt1 125.9(2) . .
C11 N1 Pt1 114.8(2) . .
C12 N2 C16 119.5(3) . .
C12 N2 Pt1 126.4(2) . .
C16 N2 Pt1 114.1(2) . .
C17 N3 Pt1 177.8(3) . .
O4 Cl1 O3 109.97(19) . .
O4 Cl1 O2 109.90(17) . .
O3 Cl1 O2 109.45(18) . .
O4 Cl1 O5 110.75(18) . .
O3 Cl1 O5 107.73(19) . .
O2 Cl1 O5 108.99(18) . .
C1 Pt1 N1 80.13(12) . .
C1 Pt1 N2 80.98(12) . .
N1 Pt1 N2 161.10(10) . .
C1 Pt1 N3 179.09(11) . .
N1 Pt1 N3 99.34(10) . .
N2 Pt1 N3 99.55(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.383(4) .
C1 C6 1.400(4) .
C1 Pt1 1.911(3) .
C2 C3 1.401(4) .
C2 C11 1.469(4) .
C3 C4 1.382(5) .
C3 H15 0.9500 .
C4 C5 1.401(5) .
C4 H14 0.9500 .
C5 C6 1.389(4) .
C5 H13 0.9500 .
C6 C16 1.468(4) .
C7 N1 1.346(4) .
C7 C8 1.381(5) .
C7 H1 0.9500 .
C8 C9 1.381(5) .
C8 H2 0.9500 .
C9 C10 1.381(5) .
C9 H3 0.9500 .
C10 C11 1.384(4) .
C10 H4 0.9500 .
C11 N1 1.378(4) .
C12 N2 1.337(4) .
C12 C13 1.382(4) .
C12 H100 0.9500 .
C13 C14 1.379(5) .
C13 H10 0.9500 .
C14 C15 1.390(5) .
C14 H11 0.9500 .
C15 C16 1.387(4) .
C15 H12 0.9500 .
C16 N2 1.371(4) .
C17 N3 1.138(4) .
C17 C18 1.455(5) .
C18 H17A 0.9800 .
C18 H17B 0.9800 .
C18 H17C 0.9800 .
C19 C20 1.415(8) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 N4 1.166(8) .
C20 N4 1.166(8) 3_666
C20 C19 1.415(8) 3_666
N1 Pt1 2.035(3) .
N2 Pt1 2.042(3) .
N3 Pt1 2.104(3) .
O2 Cl1 1.432(3) .
O3 Cl1 1.421(3) .
O4 Cl1 1.417(2) .
O5 Cl1 1.433(3) .
