#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:41:07 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232249 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/72/4347294.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_4347294
loop_
_publ_author_name
'Otake, Ken-ichi'
'Otsubo, Kazuya'
'Sugimoto, Kunihisa'
'Fujiwara, Akihiko'
'Kitagawa, Hiroshi'
_publ_section_title
;
 Neutral-Type One-Dimensional Mixed-Valence Halogen-Bridged Platinum Chain
 Complexes with Large Charge-Transfer Band Gaps.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2620
_journal_page_last               2626
_journal_paper_doi               10.1021/acs.inorgchem.5b02980
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H14 Cl N4 Pt'
_chemical_formula_sum            'C8 H14 Cl N4 Pt'
_chemical_formula_weight         396.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   5.4246(3)
_cell_length_b                   10.0714(5)
_cell_length_c                   10.7447(6)
_cell_measurement_reflns_used    3994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.77
_cell_volume                     587.02(5)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/3 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6039
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.806
_diffrn_reflns_theta_min         2.772
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.101
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             370.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.51
_refine_ls_abs_structure_details
;
 Flack x determined using 545 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.049(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0199P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0402
_reflns_Friedel_coverage         0.665
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1416
_reflns_number_total             1538
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic5b02980_si_005.cif
_cod_data_source_block           complex5
_cod_database_code               4347294
_shelxl_version_number           2014-3
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,+Z
3 1/2+X,1/2-Y,-Z
4 1/2-X,1/2+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pt1 Pt 0.5000 1.0000 0.99398(2) 0.01946(8) Uani 1 2 d S T P
Cl2 Cl 0.0719(4) 1.0074(4) 1.00117(13) 0.0291(5) Uani 0.5 1 d . . P
N1 N 0.5172(12) 1.2210(3) 1.1947(3) 0.0309(8) Uani 1 1 d . . .
N2 N 0.483(2) 0.8653(3) 0.8478(3) 0.0267(10) Uani 1 1 d . . .
H2A H 0.6301 0.8223 0.8404 0.032 Uiso 1 1 calc R U .
H2B H 0.3643 0.8037 0.8632 0.032 Uiso 1 1 calc R U .
C1 C 0.513(2) 1.1386(4) 1.1229(4) 0.0246(9) Uani 1 1 d . . .
C2 C 0.4265(7) 0.9366(4) 0.7303(4) 0.0287(10) Uani 1 1 d . . .
H2 H 0.2475 0.9604 0.7312 0.034 Uiso 1 1 calc R U .
C3 C 0.4757(15) 0.8535(4) 0.6150(4) 0.0377(12) Uani 1 1 d . . .
H3A H 0.3695 0.7736 0.6160 0.045 Uiso 1 1 calc R U .
H3B H 0.6498 0.8242 0.6145 0.045 Uiso 1 1 calc R U .
C4 C 0.4221(13) 0.9358(8) 0.4982(3) 0.0448(15) Uani 1 1 d . . .
H4A H 0.2448 0.9589 0.4955 0.054 Uiso 1 1 calc R U .
H4B H 0.4611 0.8827 0.4231 0.054 Uiso 1 1 calc R U .
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Pt Pt -1.7033 8.3905
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 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
C1 Pt1 C1 90.5(2) . 2_675
C1 Pt1 N2 93.87(16) . 2_675
C1 Pt1 N2 175.57(14) 2_675 2_675
C1 Pt1 N2 175.57(14) . .
C1 Pt1 N2 93.87(16) 2_675 .
N2 Pt1 N2 81.76(19) 2_675 .
C1 Pt1 Cl2 89.4(4) . .
C1 Pt1 Cl2 88.0(4) 2_675 .
N2 Pt1 Cl2 92.8(3) 2_675 .
N2 Pt1 Cl2 90.1(3) . .
C1 Pt1 Cl2 88.0(4) . 2_675
C1 Pt1 Cl2 89.4(4) 2_675 2_675
N2 Pt1 Cl2 90.1(3) 2_675 2_675
N2 Pt1 Cl2 92.8(3) . 2_675
Cl2 Pt1 Cl2 176.19(7) . 2_675
Cl2 Cl2 Pt1 167.3(7) 2_575 .
C2 N2 Pt1 109.6(3) . .
C2 N2 H2A 109.7 . .
Pt1 N2 H2A 109.7 . .
C2 N2 H2B 109.7 . .
Pt1 N2 H2B 109.7 . .
H2A N2 H2B 108.2 . .
N1 C1 Pt1 178.0(5) . .
N2 C2 C2 107.5(4) . 2_675
N2 C2 C3 113.0(4) . .
C2 C2 C3 112.0(3) 2_675 .
N2 C2 H2 108.1 . .
C2 C2 H2 108.1 2_675 .
C3 C2 H2 108.1 . .
C2 C3 C4 109.7(4) . .
C2 C3 H3A 109.7 . .
C4 C3 H3A 109.7 . .
C2 C3 H3B 109.7 . .
C4 C3 H3B 109.7 . .
H3A C3 H3B 108.2 . .
C3 C4 C4 110.4(5) . 2_675
C3 C4 H4A 109.6 . .
C4 C4 H4A 109.6 2_675 .
C3 C4 H4B 109.6 . .
C4 C4 H4B 109.6 2_675 .
H4A C4 H4B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C1 1.968(4) .
Pt1 C1 1.968(4) 2_675
Pt1 N2 2.078(3) 2_675
Pt1 N2 2.078(3) .
Pt1 Cl2 2.325(2) .
Pt1 Cl2 2.325(2) 2_675
Cl2 Cl2 0.794(4) 2_575
N1 C1 1.133(5) .
N2 C2 1.484(5) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
C2 C2 1.506(8) 2_675
C2 C3 1.518(5) .
C2 H2 1.0000 .
C3 C4 1.532(7) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C4 1.545(15) 2_675
C4 H4A 0.9900 .
C4 H4B 0.9900 .
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
_geom_torsion_site_symmetry_4
Pt1 N2 C2 C2 41.0(7) . 2_675
Pt1 N2 C2 C3 165.0(5) . .
N2 C2 C3 C4 -177.8(7) . .
C2 C2 C3 C4 -56.3(7) 2_675 .
C2 C3 C4 C4 56.8(8) . 2_675
