#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/72/4337205.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_4337205
loop_
_publ_author_name
'Otsubo, Kazuya'
'Kobayashi, Atsushi'
'Sugimoto, Kunihisa'
'Fujiwara, Akihiko'
'Kitagawa, Hiroshi'
_publ_section_title
;
 Variable-rung design for a mixed-valence two-legged ladder system
 situated in a dimensional crossover region.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1229
_journal_page_last               1240
_journal_paper_doi               10.1021/ic402846v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C24 H50 Cl4 N14 O16 Pt2 '
_chemical_formula_sum            'C24 H50 Cl4 N14 O16 Pt2'
_chemical_formula_weight         1322.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.1140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.0452(18)
_cell_length_b                   11.1313(14)
_cell_length_c                   15.0297(19)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.48
_cell_volume                     2192.0(5)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'CrystalStructure 3.8.0'
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  'SHELXL (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Giacovazzo, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD detector'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode with a mirror focusing unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11065
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    6.698
_exptl_absorpt_correction_T_max  0.4332
_exptl_absorpt_correction_T_min  0.1353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.348
_refine_diff_density_min         -2.580
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0374
_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)+(0.0574P)²+8.9758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                4570
_reflns_number_total             4699
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic402846v_si_002.cif
_cod_data_source_block           {[PtCl2(dien)]2(azpy)}(NO3)4_2(C3H6O)_2(H2O)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_formula_sum        'C24 H50 Cl4 N14 O16 Pt2 '
_cod_database_code               4337205
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+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 0.906754(12) 0.462556(15) 0.209653(12) 0.01474(10) Uani 1 1 d .
Cl1 Cl 1.06315(10) 0.46188(10) 0.19216(10) 0.0193(3) Uani 1 1 d .
Cl2 Cl 0.74896(10) 0.46443(10) 0.22741(10) 0.0207(3) Uani 1 1 d .
O1 O 0.9906(3) 0.3128(4) -0.0422(3) 0.0291(8) Uani 1 1 d .
O2 O 1.1185(3) 0.1929(4) 0.0202(4) 0.0416(11) Uani 1 1 d .
O3 O 0.9901(3) 0.1893(4) 0.0685(3) 0.0289(8) Uani 1 1 d .
O4 O 1.1073(4) 0.4422(4) 0.5217(4) 0.0427(12) Uani 1 1 d .
O5 O 1.1966(6) 0.3307(7) 0.4637(5) 0.083(3) Uani 1 1 d .
O6 O 1.1785(4) 0.2793(5) 0.5923(3) 0.0440(12) Uani 1 1 d .
O7 O 0.3322(4) 0.3780(5) 0.1927(3) 0.0468(12) Uani 1 1 d .
O8 O 0.3373(3) 0.1451(5) 0.0674(4) 0.0414(11) Uani 1 1 d .
H24 H 0.3070 0.0780 0.0340 0.050 Uiso 1 1 d .
H25 H 0.2790 0.1440 0.0660 0.050 Uiso 1 1 d .
N1 N 0.9463(3) 0.3138(4) 0.2990(3) 0.0168(8) Uani 1 1 d .
N2 N 1.0198(3) 0.0040(4) 0.4690(3) 0.0208(8) Uani 1 1 d .
N3 N 0.8432(3) 0.3654(4) 0.0862(3) 0.0186(8) Uani 1 1 d .
H5 H 0.8903 0.3120 0.0797 0.022 Uiso 1 1 calc R
H6 H 0.7880 0.3226 0.0881 0.022 Uiso 1 1 calc R
N4 N 0.8663(3) 0.6058(4) 0.1213(3) 0.0158(8) Uani 1 1 d .
H11 H 0.9206 0.6235 0.1020 0.019 Uiso 1 1 calc R
N5 N 0.9586(3) 0.5897(4) 0.3158(3) 0.0205(9) Uani 1 1 d .
H16 H 0.9218 0.5856 0.3554 0.025 Uiso 1 1 calc R
H17 H 1.0262 0.5760 0.3517 0.025 Uiso 1 1 calc R
N6 N 1.0339(3) 0.2309(4) 0.0155(3) 0.0236(9) Uani 1 1 d .
N7 N 1.1641(4) 0.3524(4) 0.5277(4) 0.0276(10) Uani 1 1 d .
C1 C 0.9253(4) 0.3102(4) 0.3795(3) 0.0192(9) Uani 1 1 d .
H1 H 0.8944 0.3782 0.3962 0.023 Uiso 1 1 calc R
C2 C 0.9471(4) 0.2114(4) 0.4387(3) 0.0184(9) Uani 1 1 d .
H2 H 0.9315 0.2108 0.4952 0.022 Uiso 1 1 calc R
C3 C 0.9925(4) 0.1119(4) 0.4135(3) 0.0178(9) Uani 1 1 d .
C4 C 1.0168(4) 0.1156(5) 0.3313(4) 0.0214(10) Uani 1 1 d .
H3 H 1.0492 0.0494 0.3140 0.026 Uiso 1 1 calc R
C5 C 0.9924(4) 0.2181(5) 0.2757(3) 0.0198(9) Uani 1 1 d .
H4 H 1.0083 0.2216 0.2194 0.024 Uiso 1 1 calc R
C6 C 0.8101(4) 0.4511(4) 0.0034(4) 0.0225(11) Uani 1 1 d .
H7 H 0.7519 0.4166 -0.0496 0.027 Uiso 1 1 calc R
H8 H 0.8669 0.4648 -0.0197 0.027 Uiso 1 1 calc R
C7 C 0.7784(4) 0.5702(5) 0.0353(4) 0.0207(9) Uani 1 1 d .
H9 H 0.7648 0.6316 -0.0153 0.025 Uiso 1 1 calc R
H10 H 0.7161 0.5597 0.0509 0.025 Uiso 1 1 calc R
C8 C 0.8523(4) 0.7108(5) 0.1784(4) 0.0236(10) Uani 1 1 d .
H12 H 0.7895 0.7009 0.1931 0.028 Uiso 1 1 calc R
H13 H 0.8473 0.7866 0.1426 0.028 Uiso 1 1 calc R
C9 C 0.9462(4) 0.7121(5) 0.2698(4) 0.0256(11) Uani 1 1 d .
H14 H 1.0076 0.7322 0.2550 0.031 Uiso 1 1 calc R
H15 H 0.9381 0.7738 0.3140 0.031 Uiso 1 1 calc R
C10 C 0.3135(4) 0.3570(5) 0.2639(4) 0.0249(10) Uani 1 1 d .
C11 C 0.2592(5) 0.2445(5) 0.2736(4) 0.0311(12) Uani 1 1 d .
H21 H 0.1853 0.2587 0.2484 0.037 Uiso 1 1 calc R
H22 H 0.2810 0.2219 0.3410 0.037 Uiso 1 1 calc R
H23 H 0.2756 0.1795 0.2376 0.037 Uiso 1 1 calc R
C12 C 0.3410(5) 0.4416(6) 0.3451(5) 0.0346(13) Uani 1 1 d .
H18 H 0.4094 0.4224 0.3904 0.042 Uiso 1 1 calc R
H19 H 0.2915 0.4346 0.3770 0.042 Uiso 1 1 calc R
H20 H 0.3403 0.5239 0.3217 0.042 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
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Pt Pt -1.703 8.390
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
C C 0.003 0.002
;
International Tables for Crystallography
(1992, 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
N4 Pt1 N3 83.92(15) .
N4 Pt1 N5 84.49(18) .
N3 Pt1 N5 168.32(17) .
N4 Pt1 N1 179.08(16) .
N3 Pt1 N1 95.29(15) .
N5 Pt1 N1 96.28(17) .
N4 Pt1 Cl1 88.96(12) .
N3 Pt1 Cl1 90.98(12) .
N5 Pt1 Cl1 90.28(13) .
N1 Pt1 Cl1 91.54(12) .
N4 Pt1 Cl2 90.81(12) .
N3 Pt1 Cl2 89.22(12) .
N5 Pt1 Cl2 89.47(13) .
N1 Pt1 Cl2 88.70(12) .
Cl1 Pt1 Cl2 179.67(4) .
H24 O8 H25 73.1 .
C1 N1 C5 119.2(4) .
C1 N1 Pt1 120.7(3) .
C5 N1 Pt1 120.1(3) .
N2 N2 C3 113.4(5) 3_756
C6 N3 Pt1 108.6(3) .
C6 N3 H5 110.0 .
Pt1 N3 H5 110.0 .
C6 N3 H6 110.0 .
Pt1 N3 H6 110.0 .
H5 N3 H6 108.4 .
C7 N4 C8 117.8(4) .
C7 N4 Pt1 108.0(3) .
C8 N4 Pt1 107.6(3) .
C7 N4 H11 107.7 .
C8 N4 H11 107.7 .
Pt1 N4 H11 107.7 .
C9 N5 Pt1 108.4(3) .
C9 N5 H16 110.0 .
Pt1 N5 H16 110.0 .
C9 N5 H17 110.0 .
Pt1 N5 H17 110.0 .
H16 N5 H17 108.4 .
O2 N6 O1 120.2(4) .
O2 N6 O3 121.1(4) .
O1 N6 O3 118.8(4) .
O6 N7 O5 119.2(5) .
O6 N7 O4 120.1(5) .
O5 N7 O4 120.3(5) .
N1 C1 C2 122.3(5) .
N1 C1 H1 118.8 .
C2 C1 H1 118.8 .
C1 C2 C3 118.3(4) .
C1 C2 H2 120.9 .
C3 C2 H2 120.9 .
C4 C3 C2 119.9(4) .
C4 C3 N2 116.1(4) .
C2 C3 N2 123.9(4) .
C5 C4 C3 118.2(5) .
C5 C4 H3 120.9 .
C3 C4 H3 120.9 .
N1 C5 C4 122.0(4) .
N1 C5 H4 119.0 .
C4 C5 H4 119.0 .
N3 C6 C7 109.2(4) .
N3 C6 H7 109.8 .
C7 C6 H7 109.8 .
N3 C6 H8 109.8 .
C7 C6 H8 109.8 .
H7 C6 H8 108.3 .
N4 C7 C6 105.1(4) .
N4 C7 H9 110.7 .
C6 C7 H9 110.7 .
N4 C7 H10 110.7 .
C6 C7 H10 110.7 .
H9 C7 H10 108.8 .
N4 C8 C9 105.9(4) .
N4 C8 H12 110.6 .
C9 C8 H12 110.6 .
N4 C8 H13 110.6 .
C9 C8 H13 110.6 .
H12 C8 H13 108.7 .
N5 C9 C8 108.9(4) .
N5 C9 H14 109.9 .
C8 C9 H14 109.9 .
N5 C9 H15 109.9 .
C8 C9 H15 109.9 .
H14 C9 H15 108.3 .
O7 C10 C12 122.0(6) .
O7 C10 C11 121.7(5) .
C12 C10 C11 116.3(5) .
C10 C11 H21 109.5 .
C10 C11 H22 109.5 .
H21 C11 H22 109.5 .
C10 C11 H23 109.5 .
H21 C11 H23 109.5 .
H22 C11 H23 109.5 .
C10 C12 H18 109.5 .
C10 C12 H19 109.5 .
H18 C12 H19 109.5 .
C10 C12 H20 109.5 .
H18 C12 H20 109.5 .
H19 C12 H20 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 N4 2.022(4) .
Pt1 N3 2.053(4) .
Pt1 N5 2.060(4) .
Pt1 N1 2.077(4) .
Pt1 Cl1 2.3044(13) .
Pt1 Cl2 2.3258(13) .
O1 N6 1.254(6) .
O2 N6 1.239(6) .
O3 N6 1.257(6) .
O4 N7 1.261(6) .
O5 N7 1.228(7) .
O6 N7 1.227(7) .
O7 C10 1.213(7) .
O8 H24 0.9145 .
O8 H25 0.8111 .
N1 C1 1.346(6) .
N1 C5 1.356(6) .
N2 N2 1.250(9) 3_756
N2 C3 1.434(6) .
N3 C6 1.503(6) .
N3 H5 0.9200 .
N3 H6 0.9200 .
N4 C7 1.484(6) .
N4 C8 1.503(6) .
N4 H11 0.9300 .
N5 C9 1.510(7) .
N5 H16 0.9200 .
N5 H17 0.9200 .
C1 C2 1.379(7) .
C1 H1 0.9500 .
C2 C3 1.397(7) .
C2 H2 0.9500 .
C3 C4 1.395(7) .
C4 C5 1.383(7) .
C4 H3 0.9500 .
C5 H4 0.9500 .
C6 C7 1.529(7) .
C6 H7 0.9900 .
C6 H8 0.9900 .
C7 H9 0.9900 .
C7 H10 0.9900 .
C8 C9 1.524(8) .
C8 H12 0.9900 .
C8 H13 0.9900 .
C9 H14 0.9900 .
C9 H15 0.9900 .
C10 C12 1.478(8) .
C10 C11 1.500(8) .
C11 H21 0.9800 .
C11 H22 0.9800 .
C11 H23 0.9800 .
C12 H18 0.9800 .
C12 H19 0.9800 .
C12 H20 0.9800 .
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
N3 Pt1 N1 C1 -133.1(4) .
N5 Pt1 N1 C1 45.3(4) .
Cl1 Pt1 N1 C1 135.8(4) .
Cl2 Pt1 N1 C1 -44.0(4) .
N3 Pt1 N1 C5 45.8(4) .
N5 Pt1 N1 C5 -135.8(4) .
Cl1 Pt1 N1 C5 -45.3(4) .
Cl2 Pt1 N1 C5 134.9(4) .
N4 Pt1 N3 C6 3.3(3) .
N5 Pt1 N3 C6 10.6(10) .
N1 Pt1 N3 C6 -177.1(3) .
Cl1 Pt1 N3 C6 -85.5(3) .
Cl2 Pt1 N3 C6 94.2(3) .
N3 Pt1 N4 C7 26.0(3) .
N5 Pt1 N4 C7 -152.5(3) .
Cl1 Pt1 N4 C7 117.1(3) .
Cl2 Pt1 N4 C7 -63.1(3) .
N3 Pt1 N4 C8 154.2(3) .
N5 Pt1 N4 C8 -24.3(3) .
Cl1 Pt1 N4 C8 -114.7(3) .
Cl2 Pt1 N4 C8 65.1(3) .
N4 Pt1 N5 C9 -4.6(3) .
N3 Pt1 N5 C9 -11.8(10) .
N1 Pt1 N5 C9 175.9(3) .
Cl1 Pt1 N5 C9 84.4(3) .
Cl2 Pt1 N5 C9 -95.4(3) .
C5 N1 C1 C2 -1.3(7) .
Pt1 N1 C1 C2 177.6(4) .
N1 C1 C2 C3 0.0(7) .
C1 C2 C3 C4 1.4(7) .
C1 C2 C3 N2 179.5(5) .
N2 N2 C3 C4 -167.5(6) 3_756
N2 N2 C3 C2 14.4(8) 3_756
C2 C3 C4 C5 -1.5(7) .
N2 C3 C4 C5 -179.7(5) .
C1 N1 C5 C4 1.2(7) .
Pt1 N1 C5 C4 -177.7(4) .
C3 C4 C5 N1 0.2(8) .
Pt1 N3 C6 C7 -31.5(5) .
C8 N4 C7 C6 -171.0(4) .
Pt1 N4 C7 C6 -49.0(4) .
N3 C6 C7 N4 53.0(5) .
C7 N4 C8 C9 170.2(4) .
Pt1 N4 C8 C9 47.9(4) .
Pt1 N5 C9 C8 32.5(5) .
N4 C8 C9 N5 -53.1(5) .
