#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/78/1517811.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_1517811
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         'C38 H46 N10 Pt, 2(C H4 O), 2(Br)'
_chemical_formula_sum            'C40 H54 Br2 N10 O2 Pt'
_chemical_formula_weight         1061.84
_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
_cell_angle_alpha                94.084(5)
_cell_angle_beta                 109.329(5)
_cell_angle_gamma                104.174(5)
_cell_formula_units_Z            1
_cell_length_a                   8.9470(9)
_cell_length_b                   10.8626(11)
_cell_length_c                   11.7344(12)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.18
_cell_measurement_theta_min      2.54
_cell_volume                     1028.84(19)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics
'CrystaMaker (CrystalMaker Software ltd., 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '62mm x 62mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'toroidally curved graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.5214
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18390
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    5.400
_exptl_absorpt_correction_T_max  0.4483
_exptl_absorpt_correction_T_min  0.2502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.543
_refine_diff_density_min         -2.750
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0280
_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)+(0.0309P)²+1.0208P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                5091
_reflns_number_total             5918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp506256a_si_001.cif
_cod_data_source_block           3br2meoh2
_cod_depositor_comments
'Adding full bibliography for 1517806--1517811.cif.'
_cod_original_cell_volume        1028.84(18)
_cod_database_code               1517811
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
Pt1 Pt 0.0000 0.0000 0.5000 0.01397(5) Uani 1 2 d S
N1 N -0.1684(3) 0.0976(2) 0.4764(2) 0.0138(4) Uani 1 1 d .
N2 N -0.2661(3) 0.2579(2) 0.5435(2) 0.0162(5) Uani 1 1 d .
H2N H -0.3646 0.2271 0.4859 0.019 Uiso 1 1 calc R
H2M H -0.2449 0.3271 0.5966 0.019 Uiso 1 1 calc R
N3 N 0.0006(3) 0.2543(2) 0.6471(2) 0.0134(4) Uani 1 1 d .
N4 N 0.2670(3) 0.3759(2) 0.6828(2) 0.0144(4) Uani 1 1 d .
N5 N 0.1635(3) 0.1733(2) 0.5598(2) 0.0145(4) Uani 1 1 d .
H5N H 0.2521 0.1875 0.5399 0.017 Uiso 1 1 calc R
C1 C -0.3092(3) 0.0599(3) 0.3647(2) 0.0147(5) Uani 1 1 d .
C2 C -0.3056(4) 0.1220(3) 0.2660(3) 0.0214(6) Uani 1 1 d .
H2 H -0.2134 0.1922 0.2738 0.026 Uiso 1 1 calc R
C3 C -0.4364(5) 0.0809(3) 0.1570(3) 0.0279(7) Uani 1 1 d .
H3 H -0.4360 0.1243 0.0896 0.033 Uiso 1 1 calc R
C4 C -0.5696(4) -0.0237(3) 0.1441(3) 0.0284(7) Uani 1 1 d .
H4 H -0.6584 -0.0530 0.0675 0.034 Uiso 1 1 calc R
C5 C -0.5727(4) -0.0848(3) 0.2421(3) 0.0239(6) Uani 1 1 d .
H5A H -0.6638 -0.1564 0.2334 0.029 Uiso 1 1 calc R
C6 C -0.4427(4) -0.0418(3) 0.3540(3) 0.0191(6) Uani 1 1 d .
H6 H -0.4459 -0.0823 0.4227 0.023 Uiso 1 1 calc R
C7 C -0.1494(3) 0.2000(2) 0.5503(2) 0.0130(5) Uani 1 1 d .
C8 C 0.0097(3) 0.2529(3) 0.7722(2) 0.0143(5) Uani 1 1 d .
C9 C -0.0489(4) 0.3363(3) 0.8291(3) 0.0179(6) Uani 1 1 d .
H9 H -0.0949 0.3974 0.7869 0.021 Uiso 1 1 calc R
C10 C -0.0391(4) 0.3288(3) 0.9486(3) 0.0223(6) Uani 1 1 d .
H10 H -0.0807 0.3846 0.9879 0.027 Uiso 1 1 calc R
C11 C 0.0297(4) 0.2421(3) 1.0113(3) 0.0249(7) Uani 1 1 d .
H11 H 0.0362 0.2383 1.0934 0.030 Uiso 1 1 calc R
C12 C 0.0894(4) 0.1602(3) 0.9534(3) 0.0262(7) Uani 1 1 d .
H12 H 0.1382 0.1006 0.9963 0.031 Uiso 1 1 calc R
C13 C 0.0781(4) 0.1650(3) 0.8335(3) 0.0200(6) Uani 1 1 d .
H13 H 0.1174 0.1079 0.7935 0.024 Uiso 1 1 calc R
C14 C 0.1482(3) 0.2659(2) 0.6258(2) 0.0128(5) Uani 1 1 d .
C15 C 0.2314(4) 0.4964(3) 0.7086(3) 0.0168(5) Uani 1 1 d .
H15A H 0.1131 0.4793 0.6972 0.020 Uiso 1 1 calc R
H15B H 0.2548 0.5540 0.6510 0.020 Uiso 1 1 calc R
C16 C 0.3368(4) 0.5609(3) 0.8385(3) 0.0203(6) Uani 1 1 d .
H16A H 0.3087 0.5056 0.8963 0.024 Uiso 1 1 calc R
H16B H 0.3148 0.6440 0.8554 0.024 Uiso 1 1 calc R
C17 C 0.5189(4) 0.5841(3) 0.8568(3) 0.0244(7) Uani 1 1 d .
H17A H 0.5496 0.6469 0.8055 0.029 Uiso 1 1 calc R
H17B H 0.5875 0.6207 0.9436 0.029 Uiso 1 1 calc R
C18 C 0.5520(4) 0.4591(3) 0.8224(3) 0.0221(6) Uani 1 1 d .
H18A H 0.5370 0.4014 0.8818 0.027 Uiso 1 1 calc R
H18B H 0.6682 0.4772 0.8274 0.027 Uiso 1 1 calc R
C19 C 0.4381(4) 0.3917(3) 0.6944(3) 0.0184(6) Uani 1 1 d .
H19A H 0.4638 0.4432 0.6334 0.022 Uiso 1 1 calc R
H19B H 0.4550 0.3064 0.6782 0.022 Uiso 1 1 calc R
O1S O 0.3780(3) 0.2220(2) 0.4081(2) 0.0213(4) Uani 1 1 d .
H1O H 0.3577 0.2935 0.4088 0.032 Uiso 1 1 calc R
C1S C 0.2482(4) 0.1299(3) 0.3104(3) 0.0258(7) Uani 1 1 d .
H1SA H 0.2692 0.1371 0.2340 0.039 Uiso 1 1 calc R
H1SB H 0.1424 0.1466 0.3013 0.039 Uiso 1 1 calc R
H1SC H 0.2441 0.0429 0.3291 0.039 Uiso 1 1 calc R
Br1 Br 0.17344(4) 0.42608(3) 0.36584(3) 0.02300(7) 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'
Br Br -0.2901 2.4595 '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'
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 2_556 .
N5 Pt1 N1 95.45(10) 2_556 .
N5 Pt1 N1 84.55(10) . .
N5 Pt1 N1 84.55(10) 2_556 2_556
N5 Pt1 N1 95.45(10) . 2_556
N1 Pt1 N1 180.000(1) . 2_556
C7 N1 C1 118.2(2) . .
C7 N1 Pt1 123.9(2) . .
C1 N1 Pt1 117.49(17) . .
C7 N2 H2N 120.0 . .
C7 N2 H2M 120.0 . .
H2N N2 H2M 120.0 . .
C7 N3 C14 119.0(2) . .
C7 N3 C8 120.3(2) . .
C14 N3 C8 116.6(2) . .
C14 N4 C15 122.7(2) . .
C14 N4 C19 121.7(2) . .
C15 N4 C19 113.7(2) . .
C14 N5 Pt1 124.28(18) . .
C14 N5 H5N 117.9 . .
Pt1 N5 H5N 117.9 . .
C6 C1 C2 120.7(3) . .
C6 C1 N1 119.9(3) . .
C2 C1 N1 119.3(2) . .
C3 C2 C1 119.3(3) . .
C3 C2 H2 120.4 . .
C1 C2 H2 120.4 . .
C2 C3 C4 120.6(3) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C5 C4 C3 119.9(3) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 C6 120.0(3) . .
C4 C5 H5A 120.0 . .
C6 C5 H5A 120.0 . .
C1 C6 C5 119.5(3) . .
C1 C6 H6 120.2 . .
C5 C6 H6 120.2 . .
N1 C7 N2 124.7(3) . .
N1 C7 N3 119.8(3) . .
N2 C7 N3 115.5(2) . .
C13 C8 C9 120.8(3) . .
C13 C8 N3 117.7(2) . .
C9 C8 N3 121.5(3) . .
C8 C9 C10 118.8(3) . .
C8 C9 H9 120.6 . .
C10 C9 H9 120.6 . .
C11 C10 C9 121.2(3) . .
C11 C10 H10 119.4 . .
C9 C10 H10 119.4 . .
C10 C11 C12 119.3(3) . .
C10 C11 H11 120.4 . .
C12 C11 H11 120.4 . .
C13 C12 C11 120.2(3) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
C8 C13 C12 119.7(3) . .
C8 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
N5 C14 N4 125.3(2) . .
N5 C14 N3 120.2(2) . .
N4 C14 N3 114.5(2) . .
N4 C15 C16 109.7(3) . .
N4 C15 H15A 109.7 . .
C16 C15 H15A 109.7 . .
N4 C15 H15B 109.7 . .
C16 C15 H15B 109.7 . .
H15A C15 H15B 108.2 . .
C15 C16 C17 109.7(2) . .
C15 C16 H16A 109.7 . .
C17 C16 H16A 109.7 . .
C15 C16 H16B 109.7 . .
C17 C16 H16B 109.7 . .
H16A C16 H16B 108.2 . .
C18 C17 C16 110.4(2) . .
C18 C17 H17A 109.6 . .
C16 C17 H17A 109.6 . .
C18 C17 H17B 109.6 . .
C16 C17 H17B 109.6 . .
H17A C17 H17B 108.1 . .
C17 C18 C19 112.0(3) . .
C17 C18 H18A 109.2 . .
C19 C18 H18A 109.2 . .
C17 C18 H18B 109.2 . .
C19 C18 H18B 109.2 . .
H18A C18 H18B 107.9 . .
N4 C19 C18 109.6(2) . .
N4 C19 H19A 109.8 . .
C18 C19 H19A 109.8 . .
N4 C19 H19B 109.8 . .
C18 C19 H19B 109.8 . .
H19A C19 H19B 108.2 . .
C1S O1S H1O 109.5 . .
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 1.990(2) 2_556 ?
Pt1 N5 1.990(2) . yes
Pt1 N1 2.004(2) . yes
Pt1 N1 2.004(2) 2_556 ?
N1 C7 1.300(3) . yes
N1 C1 1.432(4) . yes
N2 C7 1.329(4) . yes
N2 H2N 0.8800 . ?
N2 H2M 0.8800 . ?
N3 C7 1.395(3) . yes
N3 C14 1.401(3) . yes
N3 C8 1.445(3) . yes
N4 C14 1.340(3) . yes
N4 C15 1.456(4) . yes
N4 C19 1.457(4) . yes
N5 C14 1.288(3) . yes
N5 H5N 0.8800 . ?
C1 C6 1.378(4) . ?
C1 C2 1.387(4) . ?
C2 C3 1.370(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(4) . ?
C5 H5A 0.9500 . ?
C6 H6 0.9500 . ?
C8 C13 1.377(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 C16 1.509(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.524(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.514(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.516(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
O1S C1S 1.432(4) . ?
O1S H1O 0.8400 . ?
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 Br1 0.84 2.40 3.171(2) 152.8 . yes
N5 H5N O1S 0.88 2.20 3.006(3) 152.3 . yes
N2 H2N O1S 0.88 2.16 2.961(3) 150.6 1_455 yes
N2 H2M Br1 0.88 2.57 3.332(2) 145.7 2_566 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N5 Pt1 N1 C7 142.9(2) 2_556
N5 Pt1 N1 C7 -37.1(2) .
N1 Pt1 N1 C7 -102(51) 2_556
N5 Pt1 N1 C1 -44.08(19) 2_556
N5 Pt1 N1 C1 135.92(19) .
N1 Pt1 N1 C1 71(51) 2_556
N5 Pt1 N5 C14 64(13) 2_556
N1 Pt1 N5 C14 38.4(2) .
N1 Pt1 N5 C14 -141.6(2) 2_556
C7 N1 C1 C6 -103.5(3) .
Pt1 N1 C1 C6 83.1(3) .
C7 N1 C1 C2 80.1(3) .
Pt1 N1 C1 C2 -93.3(3) .
C6 C1 C2 C3 -0.2(5) .
N1 C1 C2 C3 176.2(3) .
C1 C2 C3 C4 -1.6(5) .
C2 C3 C4 C5 1.7(6) .
C3 C4 C5 C6 0.0(5) .
C2 C1 C6 C5 1.9(5) .
N1 C1 C6 C5 -174.5(3) .
C4 C5 C6 C1 -1.8(5) .
C1 N1 C7 N2 14.5(4) .
Pt1 N1 C7 N2 -172.5(2) .
C1 N1 C7 N3 -167.3(2) .
Pt1 N1 C7 N3 5.6(3) .
C14 N3 C7 N1 43.2(4) .
C8 N3 C7 N1 -113.2(3) .
C14 N3 C7 N2 -138.6(3) .
C8 N3 C7 N2 65.0(3) .
C7 N3 C8 C13 103.7(3) .
C14 N3 C8 C13 -53.3(3) .
C7 N3 C8 C9 -76.0(3) .
C14 N3 C8 C9 127.1(3) .
C13 C8 C9 C10 -0.7(4) .
N3 C8 C9 C10 178.9(2) .
C8 C9 C10 C11 1.0(4) .
C9 C10 C11 C12 -0.4(5) .
C10 C11 C12 C13 -0.7(5) .
C9 C8 C13 C12 -0.4(4) .
N3 C8 C13 C12 -180.0(3) .
C11 C12 C13 C8 1.0(5) .
Pt1 N5 C14 N4 169.1(2) .
Pt1 N5 C14 N3 -8.2(4) .
C15 N4 C14 N5 151.8(3) .
C19 N4 C14 N5 -11.7(4) .
C15 N4 C14 N3 -30.8(4) .
C19 N4 C14 N3 165.6(3) .
C7 N3 C14 N5 -42.1(4) .
C8 N3 C14 N5 115.2(3) .
C7 N3 C14 N4 140.4(3) .
C8 N3 C14 N4 -62.3(3) .
C14 N4 C15 C16 134.5(3) .
C19 N4 C15 C16 -60.7(3) .
N4 C15 C16 C17 57.9(3) .
C15 C16 C17 C18 -55.3(3) .
C16 C17 C18 C19 53.6(3) .
C14 N4 C19 C18 -137.4(3) .
C15 N4 C19 C18 57.7(3) .
C17 C18 C19 N4 -53.5(3) .
