#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/78/1517809.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_1517809
loop_
_publ_author_name
'Gushchin, Pavel V.'
'Kuznetsov, Maxim L.'
'Haukka, Matti'
'Kukushkin, Vadim Yu'
_publ_section_title
;
 Anionic halide···alcohol clusters in the solid
 state.
;
_journal_issue                   40
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              9529
_journal_page_last               9539
_journal_paper_doi               10.1021/jp506256a
_journal_volume                  118
_journal_year                    2014
_chemical_formula_moiety         'C36 H42 N10 O2 Pt, 2(C H4 O), 2(Cl)'
_chemical_formula_sum            'C38 H50 Cl2 N10 O4 Pt'
_chemical_formula_weight         976.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.5720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8123(5)
_cell_length_b                   21.8035(13)
_cell_length_c                   10.7171(6)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.11
_cell_measurement_theta_min      2.40
_cell_volume                     1983.6(2)
_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.3.2f (Brandenburg, 2010)'
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16376
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    3.726
_exptl_absorpt_correction_T_max  0.6160
_exptl_absorpt_correction_T_min  0.3386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0202P)²+1.7748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0455
_reflns_number_gt                4409
_reflns_number_total             5243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp506256a_si_001.cif
_cod_data_source_block           4cl2meoh2
_cod_depositor_comments
'Adding full bibliography for 1517806--1517811.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1517809
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pt1 Pt 0.5000 0.5000 0.5000 0.01274(3) Uani 1 2 d S
Cl1 Cl 0.71657(6) 0.56661(2) 0.94476(5) 0.02149(10) Uani 1 1 d .
O1 O 0.10184(19) 0.66645(7) -0.03884(14) 0.0250(3) Uani 1 1 d .
O1S O 0.92929(18) 0.55136(7) 0.75513(14) 0.0229(3) Uani 1 1 d .
H1O H 0.8996 0.5531 0.8214 0.034 Uiso 1 1 d R
N5 N 0.3527(2) 0.52713(8) 0.33341(15) 0.0159(3) Uani 1 1 d .
H5 H 0.2555 0.5167 0.3044 0.024 Uiso 1 1 d R
N3 N 0.55504(19) 0.57278(7) 0.26080(15) 0.0140(3) Uani 1 1 d .
N1 N 0.3456(2) 0.51163(7) 0.60644(16) 0.0148(3) Uani 1 1 d .
N4 N 0.2945(2) 0.58810(8) 0.14696(16) 0.0174(3) Uani 1 1 d .
N2 N 0.7767(2) 0.52156(8) 0.23665(16) 0.0169(3) Uani 1 1 d .
H2N H 0.8438 0.4904 0.2372 0.025 Uiso 1 1 d R
H2M H 0.7593 0.5387 0.1610 0.025 Uiso 1 1 d R
C14 C 0.3948(2) 0.56027(9) 0.24785(17) 0.0156(4) Uani 1 1 d .
C7 C 0.6653(2) 0.52512(9) 0.29968(17) 0.0144(4) Uani 1 1 d .
C19 C 0.1261(2) 0.59136(10) 0.1342(2) 0.0216(4) Uani 1 1 d .
H19A H 0.1055 0.5852 0.2197 0.026 Uiso 1 1 calc R
H19B H 0.0705 0.5588 0.0748 0.026 Uiso 1 1 calc R
C18 C 0.0667(3) 0.65413(10) 0.0807(2) 0.0225(4) Uani 1 1 d .
H18A H -0.0487 0.6561 0.0677 0.027 Uiso 1 1 calc R
H18B H 0.1158 0.6860 0.1445 0.027 Uiso 1 1 calc R
C16 C 0.2675(3) 0.66357(10) -0.0232(2) 0.0233(4) Uani 1 1 d .
H16A H 0.3207 0.6952 0.0398 0.028 Uiso 1 1 calc R
H16B H 0.2899 0.6725 -0.1070 0.028 Uiso 1 1 calc R
C15 C 0.3324(3) 0.60100(10) 0.02405(18) 0.0195(4) Uani 1 1 d .
H15A H 0.2849 0.5694 -0.0410 0.023 Uiso 1 1 calc R
H15B H 0.4480 0.6004 0.0372 0.023 Uiso 1 1 calc R
C8 C 0.6031(2) 0.63657(9) 0.28286(18) 0.0148(4) Uani 1 1 d .
C13 C 0.5548(3) 0.66831(10) 0.37773(19) 0.0217(4) Uani 1 1 d .
H13 H 0.4931 0.6484 0.4260 0.026 Uiso 1 1 calc R
C12 C 0.5975(3) 0.72951(11) 0.4014(2) 0.0281(5) Uani 1 1 d .
H12 H 0.5629 0.7516 0.4651 0.034 Uiso 1 1 calc R
C11 C 0.6896(3) 0.75854(10) 0.3335(2) 0.0263(5) Uani 1 1 d .
H11 H 0.7203 0.8001 0.3515 0.032 Uiso 1 1 calc R
C10 C 0.7369(3) 0.72642(10) 0.2387(2) 0.0250(5) Uani 1 1 d .
H10 H 0.8007 0.7461 0.1920 0.030 Uiso 1 1 calc R
C9 C 0.6915(3) 0.66540(9) 0.2113(2) 0.0199(4) Uani 1 1 d .
H9 H 0.7210 0.6440 0.1443 0.024 Uiso 1 1 calc R
C1 C 0.2623(2) 0.56884(9) 0.58618(18) 0.0166(4) Uani 1 1 d .
C6 C 0.1225(3) 0.57404(10) 0.4895(2) 0.0242(4) Uani 1 1 d .
H6 H 0.0724 0.5386 0.4453 0.029 Uiso 1 1 calc R
C5 C 0.0563(3) 0.63176(12) 0.4578(2) 0.0329(6) Uani 1 1 d .
H5A H -0.0383 0.6359 0.3902 0.039 Uiso 1 1 calc R
C4 C 0.1267(3) 0.68314(11) 0.5237(2) 0.0332(6) Uani 1 1 d .
H4 H 0.0812 0.7225 0.5012 0.040 Uiso 1 1 calc R
C3 C 0.2641(3) 0.67717(10) 0.6231(2) 0.0284(5) Uani 1 1 d .
H3 H 0.3112 0.7124 0.6701 0.034 Uiso 1 1 calc R
C2 C 0.3328(3) 0.62016(10) 0.65393(19) 0.0213(4) Uani 1 1 d .
H2 H 0.4277 0.6162 0.7212 0.026 Uiso 1 1 calc R
C1S C 0.8586(3) 0.60309(12) 0.6797(3) 0.0383(6) Uani 1 1 d .
H1SA H 0.7547 0.6108 0.6934 0.057 Uiso 1 1 calc R
H1SB H 0.8471 0.5947 0.5878 0.057 Uiso 1 1 calc R
H1SC H 0.9256 0.6392 0.7062 0.057 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'
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
N5 Pt1 N5 180.0 3_666 .
N5 Pt1 N1 95.37(7) 3_666 3_666
N5 Pt1 N1 84.63(7) . 3_666
N5 Pt1 N1 84.63(7) 3_666 .
N5 Pt1 N1 95.37(7) . .
N1 Pt1 N1 180.0 3_666 .
C18 O1 C16 110.45(16) . .
C1S O1S H1O 105.1 . .
C14 N5 Pt1 123.87(14) . .
C14 N5 H5 109.8 . .
Pt1 N5 H5 126.2 . .
C7 N3 C14 118.73(16) . .
C7 N3 C8 120.68(16) . .
C14 N3 C8 116.21(16) . .
C7 N1 C1 120.56(17) 3_666 .
C7 N1 Pt1 123.95(14) 3_666 .
C1 N1 Pt1 114.86(12) . .
C14 N4 C19 122.13(17) . .
C14 N4 C15 123.28(17) . .
C19 N4 C15 112.19(16) . .
C7 N2 H2N 127.7 . .
C7 N2 H2M 118.5 . .
H2N N2 H2M 106.4 . .
N5 C14 N4 124.71(19) . .
N5 C14 N3 120.50(17) . .
N4 C14 N3 114.67(17) . .
N1 C7 N2 124.65(19) 3_666 .
N1 C7 N3 119.48(18) 3_666 .
N2 C7 N3 115.87(17) . .
N4 C19 C18 108.57(17) . .
N4 C19 H19A 110.0 . .
C18 C19 H19A 110.0 . .
N4 C19 H19B 110.0 . .
C18 C19 H19B 110.0 . .
H19A C19 H19B 108.4 . .
O1 C18 C19 111.92(18) . .
O1 C18 H18A 109.2 . .
C19 C18 H18A 109.2 . .
O1 C18 H18B 109.2 . .
C19 C18 H18B 109.2 . .
H18A C18 H18B 107.9 . .
O1 C16 C15 111.25(18) . .
O1 C16 H16A 109.4 . .
C15 C16 H16A 109.4 . .
O1 C16 H16B 109.4 . .
C15 C16 H16B 109.4 . .
H16A C16 H16B 108.0 . .
N4 C15 C16 108.40(17) . .
N4 C15 H15A 110.0 . .
C16 C15 H15A 110.0 . .
N4 C15 H15B 110.0 . .
C16 C15 H15B 110.0 . .
H15A C15 H15B 108.4 . .
C9 C8 C13 120.59(19) . .
C9 C8 N3 121.84(17) . .
C13 C8 N3 117.55(18) . .
C8 C13 C12 119.4(2) . .
C8 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
C11 C12 C13 120.8(2) . .
C11 C12 H12 119.6 . .
C13 C12 H12 119.6 . .
C12 C11 C10 119.3(2) . .
C12 C11 H11 120.3 . .
C10 C11 H11 120.3 . .
C11 C10 C9 120.6(2) . .
C11 C10 H10 119.7 . .
C9 C10 H10 119.7 . .
C8 C9 C10 119.3(2) . .
C8 C9 H9 120.4 . .
C10 C9 H9 120.4 . .
C6 C1 C2 120.60(19) . .
C6 C1 N1 120.06(18) . .
C2 C1 N1 118.91(18) . .
C1 C6 C5 119.2(2) . .
C1 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
C4 C5 C6 120.6(2) . .
C4 C5 H5A 119.7 . .
C6 C5 H5A 119.7 . .
C5 C4 C3 119.8(2) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C2 C3 C4 120.2(2) . .
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 . .
C3 C2 C1 119.6(2) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
O1S C1S H1SA 109.5 . .
O1S C1S H1SB 109.5 . .
H1SA C1S H1SB 109.5 . .
O1S C1S H1SC 109.5 . .
H1SA C1S H1SC 109.5 . .
H1SB C1S H1SC 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 N5 1.9945(16) 3_666 ?
Pt1 N5 1.9945(16) . yes
Pt1 N1 2.0124(17) 3_666 ?
Pt1 N1 2.0124(17) . yes
O1 C18 1.422(2) . yes
O1 C16 1.426(3) . yes
O1S C1S 1.430(3) . ?
O1S H1O 0.8211 . ?
N5 C14 1.297(2) . yes
N5 H5 0.8603 . ?
N3 C7 1.407(3) . yes
N3 C14 1.408(3) . yes
N3 C8 1.455(2) . yes
N1 C7 1.310(3) 3_666 yes
N1 C1 1.434(2) . yes
N4 C14 1.344(2) . yes
N4 C19 1.455(3) . yes
N4 C15 1.471(2) . yes
N2 C7 1.335(3) . yes
N2 H2N 0.9001 . ?
N2 H2M 0.8687 . ?
C7 N1 1.310(3) 3_666 ?
C19 C18 1.521(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C16 C15 1.513(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C8 C9 1.382(3) . ?
C8 C13 1.388(3) . ?
C13 C12 1.391(3) . ?
C13 H13 0.9500 . ?
C12 C11 1.381(3) . ?
C12 H12 0.9500 . ?
C11 C10 1.386(3) . ?
C11 H11 0.9500 . ?
C10 C9 1.398(3) . ?
C10 H10 0.9500 . ?
C9 H9 0.9500 . ?
C1 C6 1.386(3) . ?
C1 C2 1.387(3) . ?
C6 C5 1.390(3) . ?
C6 H6 0.9500 . ?
C5 C4 1.380(3) . ?
C5 H5A 0.9500 . ?
C4 C3 1.387(3) . ?
C4 H4 0.9500 . ?
C3 C2 1.383(3) . ?
C3 H3 0.9500 . ?
C2 H2 0.9500 . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
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
O1S H1O Cl1 0.82 2.36 3.1305(16) 156.0 . yes
N5 H5 O1S 0.86 2.17 2.956(2) 152.2 3_666 yes
N2 H2N O1S 0.90 2.18 3.021(2) 155.6 3_766 yes
N2 H2M Cl1 0.87 2.33 3.1846(17) 169.6 1_554 yes
