#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:42:32 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232254 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/72/4347299.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_4347299
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 Br N4 Pt'
_chemical_formula_sum            'C8 H14 Br N4 Pt'
_chemical_formula_weight         441.22
_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                   5.5648(11)
_cell_length_b                   9.958(2)
_cell_length_c                   10.755(2)
_cell_measurement_reflns_used    4393
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.79
_cell_volume                     596.0(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.965
_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  0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6786
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.405
_diffrn_reflns_theta_min         1.893
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.058
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             406.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.84
_refine_diff_density_min         -0.86
_refine_ls_abs_structure_details
;
 Flack x determined using 474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0118
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0109P)²+0.3415P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0295
_refine_ls_wR_factor_ref         0.0301
_reflns_Friedel_coverage         0.625
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                1302
_reflns_number_total             1417
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic5b02980_si_007.cif
_cod_data_source_block           complex6
_cod_database_code               4347299
_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 1.0000 1.0000 0.99796(2) 0.01433(6) Uani 1 2 d S T P
Br1 Br 0.55284(9) 1.00392(15) 1.01308(5) 0.01746(17) Uani 0.5 1 d . . P
N1 N 1.0136(7) 1.2227(3) 1.1984(2) 0.0226(6) Uani 1 1 d . . .
N2 N 0.9895(17) 0.8627(2) 0.8513(2) 0.0199(6) Uani 1 1 d D . .
H2A H 1.1348 0.8217 0.8436 0.024 Uiso 1 1 calc DR U .
H2B H 0.8769 0.7986 0.8670 0.024 Uiso 1 1 calc DR U .
C1 C 1.0086(18) 1.1406(3) 1.1284(3) 0.0194(7) Uani 1 1 d . . .
C2 C 0.9289(6) 0.9350(3) 0.7334(3) 0.0202(8) Uani 1 1 d . . .
H2 H 0.7539 0.9578 0.7351 0.024 Uiso 1 1 calc R U .
C3 C 0.9781(9) 0.8516(3) 0.6178(3) 0.0274(8) Uani 1 1 d . . .
H3A H 0.8754 0.7705 0.6184 0.033 Uiso 1 1 calc R U .
H3B H 1.1482 0.8224 0.6173 0.033 Uiso 1 1 calc R U .
C4 C 0.9257(9) 0.9347(4) 0.5014(3) 0.0331(9) Uani 1 1 d . . .
H4A H 0.7524 0.9569 0.4983 0.040 Uiso 1 1 calc R U .
H4B H 0.9654 0.8813 0.4265 0.040 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)
;
Br Br -0.2901 2.4595
;
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 89.92(17) . 2_775
C1 Pt1 N2 175.97(10) . .
C1 Pt1 N2 94.10(12) 2_775 .
C1 Pt1 N2 94.10(12) . 2_775
C1 Pt1 N2 175.97(10) 2_775 2_775
N2 Pt1 N2 81.89(14) . 2_775
C1 Pt1 Br1 88.1(3) . .
C1 Pt1 Br1 86.6(3) 2_775 .
N2 Pt1 Br1 91.8(3) . .
N2 Pt1 Br1 93.8(3) 2_775 .
C1 Pt1 Br1 86.6(3) . 2_775
C1 Pt1 Br1 88.1(3) 2_775 2_775
N2 Pt1 Br1 93.8(3) . 2_775
N2 Pt1 Br1 91.8(3) 2_775 2_775
Br1 Pt1 Br1 172.52(2) . 2_775
Br1 Br1 Pt1 170.8(3) 2_675 .
C2 N2 Pt1 109.4(2) . .
C2 N2 H2A 109.8 . .
Pt1 N2 H2A 109.8 . .
C2 N2 H2B 109.8 . .
Pt1 N2 H2B 109.8 . .
H2A N2 H2B 108.2 . .
N1 C1 Pt1 177.6(3) . .
N2 C2 C2 107.0(3) . 2_775
N2 C2 C3 113.0(3) . .
C2 C2 C3 111.8(2) 2_775 .
N2 C2 H2 108.3 . .
C2 C2 H2 108.3 2_775 .
C3 C2 H2 108.3 . .
C2 C3 C4 109.9(3) . .
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 110.7(3) . 2_775
C3 C4 H4A 109.5 . .
C4 C4 H4A 109.5 2_775 .
C3 C4 H4B 109.5 . .
C4 C4 H4B 109.5 2_775 .
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 1.983(3) .
Pt1 C1 1.983(3) 2_775
Pt1 N2 2.088(2) .
Pt1 N2 2.088(2) 2_775
Pt1 Br1 2.4940(7) .
Pt1 Br1 2.4940(7) 2_775
Br1 Br1 0.5933(10) 2_675
N1 C1 1.112(4) .
N2 C2 1.496(4) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
C2 C2 1.517(6) 2_775
C2 C3 1.520(4) .
C2 H2 1.0000 .
C3 C4 1.529(5) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C4 1.542(9) 2_775
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 42.0(6) . 2_775
Pt1 N2 C2 C3 165.5(4) . .
N2 C2 C3 C4 -176.8(5) . .
C2 C2 C3 C4 -55.9(5) 2_775 .
C2 C3 C4 C4 56.5(5) . 2_775
