#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:35:03 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185275 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/55/7225553.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_7225553
loop_
_publ_author_name
'Ivanov, Daniil M.'
'Novikov, Alexander S.'
'Starova, Galina L.'
'Haukka, Matti'
'Kukushkin, Vadim Yu.'
_publ_section_title
;
 A family of heterotetrameric clusters of chloride species and
 halomethanes held by two halogen and two hydrogen bonds
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              5278
_journal_paper_doi               10.1039/C6CE01179A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C30 H22 Cl N5 Pt, C H Cl3'
_chemical_formula_sum            'C31 H23 Cl4 N5 Pt'
_chemical_formula_weight         802.43
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-29 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                115.493(2)
_cell_angle_beta                 91.131(2)
_cell_angle_gamma                107.138(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8061(5)
_cell_length_b                   13.1997(6)
_cell_length_c                   13.2846(6)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.77
_cell_measurement_theta_min      3.02
_cell_volume                     1461.62(12)
_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.3.2g (Brandenburg, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device
'62mm x 62mm CCD camera on three-circle goniostat'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ scans and ω scans'
_diffrn_radiation_monochromator  'flat graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54027
_diffrn_reflns_theta_full        37.89
_diffrn_reflns_theta_max         37.89
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    5.197
_exptl_absorpt_correction_T_max  0.5839
_exptl_absorpt_correction_T_min  0.2250
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark red (black)'
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.564
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         15564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0208P)²+0.4121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                14156
_reflns_number_total             15564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce01179a2.cif
_cod_data_source_block           dan17fr21
_cod_depositor_comments
'Adding full bibliography for 7225552--7225554.cif.'
_cod_database_code               7225553
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
H1N H 0.7576 1.2301 0.5323 0.020 Uiso 1 1 d R
H3 H 0.7046 1.2556 0.3997 0.023 Uiso 1 1 calc R
H4 H 0.5476 1.2811 0.2850 0.027 Uiso 1 1 calc R
H5 H 0.3273 1.1305 0.1857 0.027 Uiso 1 1 calc R
H5N H 1.1215 1.2400 0.7864 0.021 Uiso 1 1 d R
H6 H 0.2682 0.9494 0.1944 0.025 Uiso 1 1 calc R
H7 H 0.4263 0.9215 0.3064 0.021 Uiso 1 1 calc R
H11 H 0.4369 0.7630 0.3595 0.018 Uiso 1 1 calc R
H12 H 0.2867 0.6011 0.1965 0.022 Uiso 1 1 calc R
H13 H 0.3587 0.4358 0.0961 0.028 Uiso 1 1 calc R
H14 H 0.5788 0.4316 0.1609 0.027 Uiso 1 1 calc R
H15 H 0.7311 0.5930 0.3228 0.020 Uiso 1 1 calc R
H18 H 1.0333 0.7550 0.5781 0.018 Uiso 1 1 calc R
H19 H 1.0475 0.6017 0.6178 0.021 Uiso 1 1 calc R
H20 H 0.8372 0.4656 0.6246 0.023 Uiso 1 1 calc R
H21 H 0.6115 0.4819 0.5916 0.024 Uiso 1 1 calc R
H22 H 0.5954 0.6306 0.5453 0.019 Uiso 1 1 calc R
H26 H 1.3383 1.2604 0.8348 0.019 Uiso 1 1 calc R
H27 H 1.5339 1.2866 0.9573 0.022 Uiso 1 1 calc R
H28 H 1.5203 1.1452 1.0225 0.025 Uiso 1 1 calc R
H29 H 1.3157 0.9750 0.9592 0.026 Uiso 1 1 calc R
H30 H 1.1235 0.9433 0.8298 0.021 Uiso 1 1 calc R
C1 C 0.67486(15) 1.07045(11) 0.44320(10) 0.0129(2) Uani 1 1 d .
C2 C 0.57925(16) 1.08646(12) 0.36697(11) 0.0143(2) Uani 1 1 d .
C3 C 0.61587(18) 1.19356(13) 0.35872(12) 0.0190(3) Uani 1 1 d .
C4 C 0.5222(2) 1.20867(14) 0.29056(13) 0.0228(3) Uani 1 1 d .
C5 C 0.39199(19) 1.11878(15) 0.23056(13) 0.0225(3) Uani 1 1 d .
C6 C 0.35650(18) 1.01159(14) 0.23636(12) 0.0207(3) Uani 1 1 d .
C7 C 0.45034(17) 0.99530(13) 0.30366(11) 0.0171(2) Uani 1 1 d .
C8 C 0.73057(15) 0.92456(11) 0.47620(10) 0.0118(2) Uani 1 1 d .
C9 C 0.70300(15) 0.79929(11) 0.45467(10) 0.0122(2) Uani 1 1 d .
C10 C 0.60019(15) 0.69549(11) 0.35779(10) 0.0126(2) Uani 1 1 d .
C11 C 0.46662(16) 0.69610(12) 0.31911(11) 0.0148(2) Uani 1 1 d .
C12 C 0.37693(17) 0.59969(13) 0.22212(12) 0.0181(2) Uani 1 1 d .
C13 C 0.41936(19) 0.50136(14) 0.16273(13) 0.0230(3) Uani 1 1 d .
C14 C 0.55057(19) 0.49931(13) 0.20106(12) 0.0222(3) Uani 1 1 d .
C15 C 0.64125(17) 0.59532(12) 0.29762(11) 0.0163(2) Uani 1 1 d .
C16 C 0.79987(15) 0.80292(11) 0.53182(10) 0.0120(2) Uani 1 1 d .
C17 C 0.81255(15) 0.70723(11) 0.55638(10) 0.0125(2) Uani 1 1 d .
C18 C 0.94733(16) 0.69878(12) 0.57927(11) 0.0151(2) Uani 1 1 d .
C19 C 0.95589(17) 0.60816(12) 0.60382(12) 0.0175(2) Uani 1 1 d .
C20 C 0.83090(18) 0.52730(12) 0.60785(12) 0.0191(3) Uani 1 1 d .
C21 C 0.69681(18) 0.53641(12) 0.58741(13) 0.0197(3) Uani 1 1 d .
C22 C 0.68744(16) 0.62545(12) 0.56070(11) 0.0162(2) Uani 1 1 d .
C23 C 0.89336(15) 0.92927(11) 0.59857(10) 0.0119(2) Uani 1 1 d .
C24 C 1.08597(15) 1.08089(11) 0.74209(10) 0.0128(2) Uani 1 1 d .
C25 C 1.21055(16) 1.09997(11) 0.82086(10) 0.0134(2) Uani 1 1 d .
C26 C 1.33385(16) 1.20185(12) 0.85930(11) 0.0156(2) Uani 1 1 d .
C27 C 1.44965(17) 1.21803(13) 0.93285(12) 0.0187(3) Uani 1 1 d .
C28 C 1.44205(19) 1.13349(14) 0.97073(12) 0.0210(3) Uani 1 1 d .
C29 C 1.32048(19) 1.03230(13) 0.93299(12) 0.0214(3) Uani 1 1 d .
C30 C 1.20540(17) 1.01399(12) 0.85703(12) 0.0174(2) Uani 1 1 d .
N1 N 0.76713(13) 1.16384(10) 0.52829(9) 0.01333(19) Uani 1 1 d .
N2 N 0.65359(13) 0.95496(10) 0.41976(9) 0.01329(19) Uani 1 1 d .
N3 N 0.84657(13) 0.99670(9) 0.56119(9) 0.01213(18) Uani 1 1 d .
N4 N 1.00030(13) 0.96404(10) 0.67869(9) 0.01347(19) Uani 1 1 d .
N5 N 1.06205(14) 1.17156(10) 0.73787(9) 0.01387(19) Uani 1 1 d .
Cl1 Cl 0.98900(4) 1.37582(3) 0.72853(3) 0.01701(6) Uani 1 1 d .
Pt1 Pt 0.914016(5) 1.170273(4) 0.635558(4) 0.01108(1) Uani 1 1 d .
H1S H 0.0535 0.4040 0.1668 0.036 Uiso 1 1 calc R
C1S C -0.0097(2) 0.32948(14) 0.10054(14) 0.0296(4) Uani 1 1 d .
Cl1S Cl 0.06480(7) 0.21688(5) 0.07558(5) 0.04519(13) Uani 1 1 d .
Cl2S Cl -0.18472(6) 0.29116(4) 0.13468(4) 0.03807(10) Uani 1 1 d .
Cl3S Cl -0.01225(10) 0.35746(5) -0.01628(5) 0.0591(2) 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'
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_publ_flag
N1 C1 C2 120.00(11) ?
N1 C1 N2 124.74(12) ?
N2 C1 C2 115.21(11) ?
C3 C2 C1 120.86(13) ?
C7 C2 C1 120.11(11) ?
C7 C2 C3 119.03(12) ?
C2 C3 H3 120.0 ?
C4 C3 H3 120.0 ?
C4 C3 C2 120.01(14) ?
C3 C4 H4 119.7 ?
C5 C4 H4 119.7 ?
C5 C4 C3 120.54(14) ?
C4 C5 H5 120.1 ?
C4 C5 C6 119.76(14) ?
C6 C5 H5 120.1 ?
C5 C6 H6 120.0 ?
C5 C6 C7 120.06(15) ?
C7 C6 H6 120.0 ?
C2 C7 H7 119.7 ?
C6 C7 H7 119.7 ?
C6 C7 C2 120.55(13) ?
N2 C8 C9 123.49(12) ?
N2 C8 N3 128.09(11) ?
N3 C8 C9 108.42(10) ?
C10 C9 C8 123.48(11) ?
C16 C9 C8 106.77(11) ?
C16 C9 C10 129.37(11) ?
C11 C10 C9 122.31(12) ?
C11 C10 C15 118.74(12) ?
C15 C10 C9 118.82(12) ?
C10 C11 H11 119.7 ?
C12 C11 H11 119.7 ?
C12 C11 C10 120.70(13) ?
C11 C12 H12 120.0 ?
C13 C12 H12 120.0 ?
C13 C12 C11 120.01(14) ?
C12 C13 H13 120.1 ?
C14 C13 H13 120.1 ?
C14 C13 C12 119.73(14) ?
C13 C14 H14 119.6 ?
C13 C14 C15 120.74(14) ?
C15 C14 H14 119.6 ?
C10 C15 H15 120.0 ?
C14 C15 H15 120.0 ?
C14 C15 C10 120.07(14) ?
C9 C16 C17 130.02(12) ?
C9 C16 C23 107.02(10) ?
C17 C16 C23 122.84(11) ?
C18 C17 C16 121.45(12) ?
C22 C17 C16 119.24(13) ?
C22 C17 C18 119.27(11) ?
C17 C18 H18 120.0 ?
C19 C18 H18 120.0 ?
C19 C18 C17 120.10(13) ?
C18 C19 H19 119.9 ?
C20 C19 H19 119.9 ?
C20 C19 C18 120.18(14) ?
C19 C20 H20 119.9 ?
C21 C20 H20 119.9 ?
C21 C20 C19 120.12(12) ?
C20 C21 H21 120.0 ?
C20 C21 C22 119.92(14) ?
C22 C21 H21 120.0 ?
C17 C22 H22 119.8 ?
C21 C22 H22 119.8 ?
C21 C22 C17 120.39(14) ?
N3 C23 C16 108.50(11) ?
N4 C23 C16 123.08(11) ?
N4 C23 N3 128.42(12) ?
N4 C24 C25 114.88(11) ?
N5 C24 C25 120.51(12) ?
N5 C24 N4 124.60(12) ?
C26 C25 C24 121.36(11) ?
C26 C25 C30 119.27(12) ?
C30 C25 C24 119.37(12) ?
C25 C26 H26 119.7 ?
C27 C26 H26 119.7 ?
C27 C26 C25 120.53(12) ?
C26 C27 H27 120.1 ?
C26 C27 C28 119.80(14) ?
C28 C27 H27 120.1 ?
C27 C28 H28 120.0 ?
C29 C28 H28 120.0 ?
C29 C28 C27 120.03(14) ?
C28 C29 H29 119.7 ?
C28 C29 C30 120.51(13) ?
C30 C29 H29 119.7 ?
C25 C30 H30 120.1 ?
C29 C30 H30 120.1 ?
C29 C30 C25 119.82(14) ?
C1 N1 H1N 110.2 ?
C1 N1 Pt1 128.94(9) ?
Pt1 N1 H1N 120.8 ?
C8 N2 C1 123.34(12) ?
C8 N3 C23 109.21(10) ?
C8 N3 Pt1 125.43(8) ?
C23 N3 Pt1 124.57(9) ?
C23 N4 C24 123.53(11) ?
C24 N5 H5N 114.0 ?
C24 N5 Pt1 128.55(9) ?
Pt1 N5 H5N 117.5 ?
N1 Pt1 Cl1 91.45(3) ?
N3 Pt1 N1 88.83(5) yes
N3 Pt1 N5 89.47(5) yes
N3 Pt1 Cl1 177.98(3) ?
N5 Pt1 N1 177.80(4) ?
N5 Pt1 Cl1 90.30(3) ?
Cl1S C1S H1S 108.1 ?
Cl1S C1S Cl2S 110.68(9) ?
Cl2S C1S H1S 108.1 ?
Cl3S C1S H1S 108.1 ?
Cl3S C1S Cl1S 110.28(10) ?
Cl3S C1S Cl2S 111.45(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 1.4874(18) ?
C2 C3 1.4055(18) ?
C2 C7 1.394(2) ?
C3 H3 0.9500 ?
C3 C4 1.391(2) ?
C4 H4 0.9500 ?
C4 C5 1.388(3) ?
C5 H5 0.9500 ?
C5 C6 1.391(2) ?
C6 H6 0.9500 ?
C6 C7 1.394(2) ?
C7 H7 0.9500 ?
C8 C9 1.4884(17) ?
C9 C10 1.4720(18) ?
C9 C16 1.3593(18) ?
C10 C11 1.401(2) ?
C10 C15 1.4021(19) ?
C11 H11 0.9500 ?
C11 C12 1.3918(19) ?
C12 H12 0.9500 ?
C12 C13 1.389(2) ?
C13 H13 0.9500 ?
C13 C14 1.386(2) ?
C14 H14 0.9500 ?
C14 C15 1.391(2) ?
C15 H15 0.9500 ?
C16 C17 1.4707(17) ?
C16 C23 1.4840(17) ?
C17 C18 1.397(2) ?
C17 C22 1.396(2) ?
C18 H18 0.9500 ?
C18 C19 1.3920(18) ?
C19 H19 0.9500 ?
C19 C20 1.387(2) ?
C20 H20 0.9500 ?
C20 C21 1.387(2) ?
C21 H21 0.9500 ?
C21 C22 1.3918(18) ?
C22 H22 0.9500 ?
C24 C25 1.4806(19) ?
C25 C26 1.3991(19) ?
C25 C30 1.3993(18) ?
C26 H26 0.9500 ?
C26 C27 1.387(2) ?
C27 H27 0.9500 ?
C27 C28 1.393(2) ?
C28 H28 0.9500 ?
C28 C29 1.385(2) ?
C29 H29 0.9500 ?
C29 C30 1.391(2) ?
C30 H30 0.9500 ?
N1 H1N 0.8856 ?
N1 C1 1.3111(17) ?
N2 C1 1.3660(16) ?
N2 C8 1.3070(16) ?
N3 C8 1.3642(17) ?
N3 C23 1.3643(16) ?
N4 C23 1.3019(17) ?
N4 C24 1.3726(17) ?
N5 H5N 0.8630 ?
N5 C24 1.3089(16) ?
Pt1 N1 1.9635(11) yes
Pt1 N3 1.9482(11) yes
Pt1 N5 1.9603(12) yes
Pt1 Cl1 2.3089(3) yes
C1S H1S 1.0000 ?
Cl1S C1S 1.755(2) ?
Cl2S C1S 1.767(2) ?
Cl3S C1S 1.7443(17) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N5 H5N Cl3S 0.86 2.97 3.3865(13) 111.7 1_666 yes
