#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/45/4334579.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_4334579
loop_
_publ_author_name
'Masayuki Kobayashi'
'Didier Savard'
'Andrew R. Geisheimer'
'Ken Sakai'
'Daniel B. Leznoff'
_publ_contact_author_address
; 
Leznoff, Daniel B.
Department of Chemistry
Simon Fraser University
Burnaby, British Columbia
Canada         V5A 1S6
;
_publ_contact_author_email       dleznoff@sfu.ca
_publ_contact_author_fax         +1-778-782-3765
_publ_contact_author_name        'Daniel B. Leznoff'
_publ_contact_author_phone       +1-778-782-4887
_publ_section_title
;
 Heterobimetallic Coordination Polymers Based on the [Pt(SCN)4]2- and
 [Pt(SeCN)4]2- Building Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4842
_journal_page_last               4852
_journal_paper_doi               10.1021/ic302360b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C8 H16 N8 Ni1 Pt1 S4'
_chemical_formula_sum            'C8 H16 N8 Ni Pt S4'
_chemical_formula_weight         606.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 111.943(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7946(18)
_cell_length_b                   11.3401(18)
_cell_length_c                   14.311(2)
_cell_measurement_reflns_used    6515
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.59
_cell_volume                     1775.5(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10000
_diffrn_reflns_theta_full        26.765
_diffrn_reflns_theta_max         27.592
_diffrn_reflns_theta_min         1.919
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.407
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.54
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3669
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.001654
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.02P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0367
_refine_ls_wR_factor_gt          0.0328
_refine_ls_wR_factor_ref         0.0323
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3734
_reflns_number_total             4032
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0243
_oxford_refine_ls_scale          0.2133(3)
_oxford_reflns_number_all        4032
_oxford_reflns_threshold_expression_ref I>2.5\s(I)
_cod_data_source_file            ic302360b_si_002_08.cif
_cod_data_source_block           C8H16N8NiPtS4
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C8 H16 N8 Ni1 Pt1 S4'
_cod_database_code               4334579
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
Pt1 Pt 0.477346(12) 0.514818(13) 0.307416(10) 0.0140 1.0000 Uani .
Ni1 Ni 1.0000 0.5000 0.5000 0.0148 1.0000 Uani S
Ni2 Ni 0.5000 1.0000 0.5000 0.0159 1.0000 Uani S
S1 S 0.59703(8) 0.68211(8) 0.32513(7) 0.0181 1.0000 Uani .
S2 S 0.36164(9) 0.59358(9) 0.39186(8) 0.0236 1.0000 Uani .
S3 S 0.36441(9) 0.34090(9) 0.27733(8) 0.0227 1.0000 Uani .
S4 S 0.58793(10) 0.43522(10) 0.21682(8) 0.0253 1.0000 Uani .
N1 N 0.8317(3) 0.5888(3) 0.4336(2) 0.0205 1.0000 Uani .
N2 N 0.4381(3) 0.8237(3) 0.4625(2) 0.0191 1.0000 Uani .
N3 N 0.1389(3) 0.3787(3) 0.3008(3) 0.0251 1.0000 Uani .
N4 N 0.6315(3) 0.1986(4) 0.2840(3) 0.0330 1.0000 Uani .
N5 N 1.0769(3) 0.6034(3) 0.4185(2) 0.0189 1.0000 Uani .
N6 N 1.0602(3) 0.6370(3) 0.6048(2) 0.0215 1.0000 Uani .
N7 N 0.6615(3) 0.9331(3) 0.6069(2) 0.0215 1.0000 Uani .
N8 N 0.5968(3) 0.9833(3) 0.4037(3) 0.0200 1.0000 Uani .
C2 C 0.4116(3) 0.7297(3) 0.4328(3) 0.0161 1.0000 Uani .
C3 C 0.2324(3) 0.3659(3) 0.2942(3) 0.0186 1.0000 Uani .
C4 C 0.6141(3) 0.2954(4) 0.2581(3) 0.0225 1.0000 Uani .
C5 C 1.1450(4) 0.7017(4) 0.4832(3) 0.0227 1.0000 Uani .
C6 C 1.0768(4) 0.7411(4) 0.5492(3) 0.0257 1.0000 Uani .
C7 C 0.7343(4) 0.8791(4) 0.5530(3) 0.0268 1.0000 Uani .
C8 C 0.7269(4) 0.9590(4) 0.4664(3) 0.0278 1.0000 Uani .
C9 C 0.7360(3) 0.6254(3) 0.3894(3) 0.0177 1.0000 Uani .
H51 H 1.0140 0.6341 0.3604 0.026(3) 1.0000 Uiso R
H52 H 1.1310 0.5568 0.3986 0.026(3) 1.0000 Uiso R
H53 H 1.1510 0.7655 0.4422 0.032(3) 1.0000 Uiso R
H54 H 1.2247 0.6759 0.5244 0.032(3) 1.0000 Uiso R
H61 H 1.1360 0.6164 0.6562 0.029(3) 1.0000 Uiso R
H62 H 1.0016 0.6525 0.6341 0.029(3) 1.0000 Uiso R
H63 H 1.1224 0.8000 0.5951 0.034(3) 1.0000 Uiso R
H64 H 0.9991 0.7719 0.5085 0.034(3) 1.0000 Uiso R
H71 H 0.6427 0.8757 0.6472 0.027(3) 1.0000 Uiso R
H72 H 0.7069 0.9954 0.6484 0.027(3) 1.0000 Uiso R
H73 H 0.7013 0.8040 0.5278 0.034(3) 1.0000 Uiso R
H74 H 0.8169 0.8703 0.5977 0.034(3) 1.0000 Uiso R
H81 H 0.5904 1.0542 0.3666 0.028(3) 1.0000 Uiso R
H82 H 0.5642 0.9197 0.3583 0.028(3) 1.0000 Uiso R
H83 H 0.7674 1.0312 0.4923 0.035(3) 1.0000 Uiso R
H84 H 0.7653 0.9219 0.4265 0.035(3) 1.0000 Uiso R
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 . Pt1 S2 . 94.63(4) yes
S1 . Pt1 S3 . 174.28(3) yes
S2 . Pt1 S3 . 90.87(4) yes
S1 . Pt1 S4 . 86.19(4) yes
S2 . Pt1 S4 . 177.94(4) yes
S3 . Pt1 S4 . 88.26(4) yes
N1 2_766 Ni1 N6 2_766 88.78(13) yes
N1 2_766 Ni1 N5 2_766 90.71(12) yes
N6 2_766 Ni1 N5 2_766 83.16(12) yes
N1 2_766 Ni1 N1 . 179.995 yes
N6 2_766 Ni1 N1 . 91.22(13) yes
N5 2_766 Ni1 N1 . 89.29(13) yes
N1 2_766 Ni1 N5 . 89.29(12) yes
N6 2_766 Ni1 N5 . 96.84(12) yes
N5 2_766 Ni1 N5 . 179.994 yes
N1 . Ni1 N5 . 90.71(12) yes
N1 2_766 Ni1 N6 . 91.22(13) yes
N6 2_766 Ni1 N6 . 179.995 yes
N5 2_766 Ni1 N6 . 96.84(13) yes
N1 . Ni1 N6 . 88.78(13) yes
N5 . Ni1 N6 . 83.16(13) yes
N2 2_676 Ni2 N8 2_676 88.23(12) yes
N2 2_676 Ni2 N7 2_676 88.65(13) yes
N8 2_676 Ni2 N7 2_676 82.96(13) yes
N2 2_676 Ni2 N2 . 179.995 yes
N8 2_676 Ni2 N2 . 91.77(12) yes
N7 2_676 Ni2 N2 . 91.35(13) yes
N2 2_676 Ni2 N7 . 91.35(13) yes
N8 2_676 Ni2 N7 . 97.04(13) yes
N7 2_676 Ni2 N7 . 179.995 yes
N2 . Ni2 N7 . 88.65(13) yes
N2 2_676 Ni2 N8 . 91.77(12) yes
N8 2_676 Ni2 N8 . 179.995 yes
N7 2_676 Ni2 N8 . 97.04(13) yes
N2 . Ni2 N8 . 88.23(12) yes
N7 . Ni2 N8 . 82.96(13) yes
Pt1 . S1 C9 . 100.13(13) yes
Pt1 . S2 C2 . 109.79(13) yes
Pt1 . S3 C3 . 109.05(14) yes
Pt1 . S4 C4 . 103.71(14) yes
Ni1 . N1 C9 . 171.5(3) yes
Ni2 . N2 C2 . 170.9(3) yes
Ni1 . N5 C5 . 108.8(2) yes
Ni1 . N5 H51 . 109.6 no
C5 . N5 H51 . 109.6 no
Ni1 . N5 H52 . 109.6 no
C5 . N5 H52 . 109.8 no
H51 . N5 H52 . 109.5 no
Ni1 . N6 C6 . 106.6(2) yes
Ni1 . N6 H61 . 110.0 no
C6 . N6 H61 . 109.7 no
Ni1 . N6 H62 . 110.3 no
C6 . N6 H62 . 110.7 no
H61 . N6 H62 . 109.5 no
Ni2 . N7 C7 . 108.4(2) yes
Ni2 . N7 H71 . 109.7 no
C7 . N7 H71 . 110.2 no
Ni2 . N7 H72 . 109.6 no
C7 . N7 H72 . 109.4 no
H71 . N7 H72 . 109.5 no
Ni2 . N8 C8 . 108.2(3) yes
Ni2 . N8 H81 . 109.9 no
C8 . N8 H81 . 110.1 no
Ni2 . N8 H82 . 109.6 no
C8 . N8 H82 . 109.6 no
H81 . N8 H82 . 109.5 no
S2 . C2 N2 . 174.9(3) yes
S3 . C3 N3 . 175.9(4) yes
S4 . C4 N4 . 178.3(4) yes
N5 . C5 C6 . 108.7(3) yes
N5 . C5 H53 . 109.6 no
C6 . C5 H53 . 109.8 no
N5 . C5 H54 . 109.6 no
C6 . C5 H54 . 109.6 no
H53 . C5 H54 . 109.5 no
C5 . C6 N6 . 107.9(3) yes
C5 . C6 H63 . 110.0 no
N6 . C6 H63 . 110.2 no
C5 . C6 H64 . 109.9 no
N6 . C6 H64 . 109.4 no
H63 . C6 H64 . 109.5 no
N7 . C7 C8 . 108.1(3) yes
N7 . C7 H73 . 109.4 no
C8 . C7 H73 . 109.7 no
N7 . C7 H74 . 109.9 no
C8 . C7 H74 . 110.2 no
H73 . C7 H74 . 109.5 no
C7 . C8 N8 . 109.7(3) yes
C7 . C8 H83 . 109.3 no
N8 . C8 H83 . 109.3 no
C7 . C8 H84 . 109.5 no
N8 . C8 H84 . 109.6 no
H83 . C8 H84 . 109.5 no
S1 . C9 N1 . 178.7(4) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 S1 . 2.3213(10) yes
Pt1 S2 . 2.3137(10) yes
Pt1 S3 . 2.3282(10) yes
Pt1 S4 . 2.3368(10) yes
Ni1 N1 2_766 2.109(3) yes
Ni1 N6 2_766 2.090(3) yes
Ni1 N5 2_766 2.085(3) yes
Ni1 N1 . 2.109(3) yes
Ni1 N5 . 2.085(3) yes
Ni1 N6 . 2.090(3) yes
Ni2 N2 2_676 2.127(3) yes
Ni2 N8 2_676 2.102(4) yes
Ni2 N7 2_676 2.089(3) yes
Ni2 N2 . 2.127(3) yes
Ni2 N7 . 2.089(3) yes
Ni2 N8 . 2.102(4) yes
S1 C9 . 1.679(4) yes
S2 C2 . 1.678(4) yes
S3 C3 . 1.686(4) yes
S4 C4 . 1.680(5) yes
N1 C9 . 1.146(5) yes
N2 C2 . 1.147(5) yes
N3 C3 . 1.151(5) yes
N4 C4 . 1.152(6) yes
N5 C5 . 1.479(5) yes
N5 H51 . 0.950 no
N5 H52 . 0.950 no
N6 C6 . 1.477(5) yes
N6 H61 . 0.950 no
N6 H62 . 0.950 no
N7 C7 . 1.484(5) yes
N7 H71 . 0.950 no
N7 H72 . 0.950 no
N8 C8 . 1.486(5) yes
N8 H81 . 0.950 no
N8 H82 . 0.950 no
C5 C6 . 1.519(5) yes
C5 H53 . 0.950 no
C5 H54 . 0.950 no
C6 H63 . 0.950 no
C6 H64 . 0.950 no
C7 C8 . 1.511(6) yes
C7 H73 . 0.950 no
C7 H74 . 0.950 no
C8 H83 . 0.950 no
C8 H84 . 0.950 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N5 H51 N4 3_655 176 0.95 2.26 3.206(6) yes
N5 H51 C4 3_655 156 0.95 2.57 3.456(6) yes
N5 H52 N3 1_655 143 0.95 2.48 3.284(6) yes
N6 H62 N3 2_666 160 0.95 2.21 3.122(6) yes
N7 H72 C3 4_565 147 0.95 2.54 3.378(6) yes
N8 H81 N4 1_565 162 0.95 2.18 3.096(6) yes
