#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/56/4315638.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_4315638
loop_
_publ_author_name
'Michael G. Fraser'
'Allan G. Blackman'
'Garth I. S. Irwin'
'Campbell P. Easton'
'Keith C. Gordon'
_publ_section_title
;
 Effect of Sulfur-Based Substituents on the Electronic Properties of Re(I)
 dppz Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5180
_journal_page_last               5189
_journal_paper_doi               10.1021/ic1003116
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C20 H8 N6 S2'
_chemical_formula_weight         396.44
_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                95.95(1)
_cell_angle_beta                 112.13(1)
_cell_angle_gamma                95.38(1)
_cell_formula_units_Z            2
_cell_length_a                   8.780(1)
_cell_length_b                   9.792(1)
_cell_length_c                   10.400(1)
_cell_measurement_reflns_used    8435
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      41.39
_cell_measurement_theta_min      2.77
_cell_volume                     815.19(16)
_computing_cell_refinement       'ApexII and SAINT (Bruker, 2001)'
_computing_data_collection       'ApexII (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'bruker Kappa ApexII area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25533
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.884893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Bronze
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Yellow
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0510P)²+0.3637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                3283
_reflns_number_total             3570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1003116_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measrured' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        815.2(2)
_cod_database_code               4315638
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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.46573(4) 0.55930(3) 1.32462(3) 0.01352(10) Uani 1 1 d . . .
S2 S 0.16158(4) 0.34116(3) 1.26967(3) 0.01501(10) Uani 1 1 d . . .
C4 C 0.64742(14) 0.09435(13) 0.78252(13) 0.0122(2) Uani 1 1 d . . .
C5 C 0.60347(15) -0.02644(13) 0.68295(13) 0.0125(2) Uani 1 1 d . . .
C12 C 0.53985(14) 0.12868(13) 0.85615(12) 0.0111(2) Uani 1 1 d . . .
N4 N 0.58521(12) 0.24370(11) 0.94941(11) 0.0119(2) Uani 1 1 d . . .
N1 N 0.70011(13) -0.06409(12) 0.61412(11) 0.0155(2) Uani 1 1 d . . .
C7 C 0.34342(14) -0.08694(13) 0.72125(13) 0.0120(2) Uani 1 1 d . . .
N3 N 0.28967(12) 0.06042(11) 0.89287(11) 0.0119(2) Uani 1 1 d . . .
C15 C 0.42651(14) 0.41585(12) 1.19086(12) 0.0116(2) Uani 1 1 d . . .
C6 C 0.44769(15) -0.11916(13) 0.65121(13) 0.0125(2) Uani 1 1 d . . .
C14 C 0.52559(14) 0.39112(13) 1.11816(13) 0.0120(2) Uani 1 1 d . . .
H27 H 0.6204 0.4531 1.1353 0.014 Uiso 1 1 calc R . .
C11 C 0.38951(14) 0.03713(13) 0.82632(13) 0.0115(2) Uani 1 1 d . . .
C3 C 0.79684(14) 0.18007(13) 0.80969(13) 0.0141(3) Uani 1 1 d . . .
H6 H 0.8296 0.2606 0.8751 0.017 Uiso 1 1 calc R . .
C16 C 0.27981(14) 0.32069(13) 1.16326(13) 0.0121(2) Uani 1 1 d . . .
C13 C 0.48222(14) 0.27003(13) 1.01646(12) 0.0114(2) Uani 1 1 d . . .
C10 C 0.26917(16) -0.31597(14) 0.52639(13) 0.0163(3) Uani 1 1 d . . .
H9 H 0.2426 -0.3947 0.4596 0.020 Uiso 1 1 calc R . .
C18 C 0.33519(14) 0.17719(13) 0.98822(12) 0.0114(2) Uani 1 1 d . . .
C17 C 0.23481(14) 0.20503(13) 1.06497(13) 0.0123(2) Uani 1 1 d . . .
H11 H 0.1389 0.1446 1.0482 0.015 Uiso 1 1 calc R . .
N2 N 0.41093(13) -0.23457(11) 0.55521(11) 0.0150(2) Uani 1 1 d . . .
C20 C 0.02897(15) 0.44827(13) 1.18163(14) 0.0176(3) Uani 1 1 d . . .
C8 C 0.19539(15) -0.17620(13) 0.68899(13) 0.0142(3) Uani 1 1 d . . .
H14 H 0.1245 -0.1576 0.7342 0.017 Uiso 1 1 calc R . .
C1 C 0.84035(15) 0.02044(14) 0.64210(14) 0.0169(3) Uani 1 1 d . . .
H15 H 0.9069 -0.0040 0.5944 0.020 Uiso 1 1 calc R . .
C2 C 0.89440(15) 0.14303(14) 0.73785(14) 0.0160(3) Uani 1 1 d . . .
H16 H 0.9934 0.1983 0.7529 0.019 Uiso 1 1 calc R . .
C9 C 0.15667(15) -0.29195(14) 0.58925(14) 0.0161(3) Uani 1 1 d . . .
H18 H 0.0585 -0.3525 0.5644 0.019 Uiso 1 1 calc R . .
C19 C 0.64769(15) 0.64031(13) 1.33060(13) 0.0158(3) Uani 1 1 d . . .
N6 N -0.06615(15) 0.51936(13) 1.12949(14) 0.0261(3) Uani 1 1 d . . .
N5 N 0.77170(14) 0.70014(13) 1.33980(13) 0.0234(3) 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
C19 S1 C15 100.44(6) . . ?
C20 S2 C16 100.48(6) . . ?
C5 C4 C3 118.36(11) . . ?
C5 C4 C12 120.52(11) . . ?
C3 C4 C12 121.12(11) . . ?
N1 C5 C4 122.78(11) . . ?
N1 C5 C6 117.11(11) . . ?
C4 C5 C6 120.11(11) . . ?
N4 C12 C11 121.96(11) . . ?
N4 C12 C4 118.87(11) . . ?
C11 C12 C4 119.17(11) . . ?
C12 N4 C13 116.64(10) . . ?
C1 N1 C5 117.05(11) . . ?
C8 C7 C6 118.86(11) . . ?
C8 C7 C11 120.73(11) . . ?
C6 C7 C11 120.41(11) . . ?
C11 N3 C18 116.45(10) . . ?
C14 C15 C16 120.05(11) . . ?
C14 C15 S1 125.29(9) . . ?
C16 C15 S1 114.65(9) . . ?
N2 C6 C7 122.17(11) . . ?
N2 C6 C5 118.05(11) . . ?
C7 C6 C5 119.78(11) . . ?
C15 C14 C13 119.54(11) . . ?
N3 C11 C12 121.92(11) . . ?
N3 C11 C7 118.07(11) . . ?
C12 C11 C7 120.00(11) . . ?
C2 C3 C4 118.97(12) . . ?
C17 C16 C15 121.36(11) . . ?
C17 C16 S2 117.76(9) . . ?
C15 C16 S2 120.59(9) . . ?
N4 C13 C14 118.95(10) . . ?
N4 C13 C18 120.97(11) . . ?
C14 C13 C18 120.07(11) . . ?
N2 C10 C9 124.71(12) . . ?
N3 C18 C17 118.65(11) . . ?
N3 C18 C13 122.03(11) . . ?
C17 C18 C13 119.29(11) . . ?
C16 C17 C18 119.67(11) . . ?
C10 N2 C6 117.31(11) . . ?
N6 C20 S2 174.74(12) . . ?
C9 C8 C7 118.84(11) . . ?
N1 C1 C2 124.64(12) . . ?
C3 C2 C1 118.19(11) . . ?
C8 C9 C10 118.09(11) . . ?
N5 C19 S1 176.71(12) . . ?
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
S1 C19 1.6920(13) . ?
S1 C15 1.7804(12) . ?
S2 C20 1.7085(14) . ?
S2 C16 1.7890(12) . ?
C4 C5 1.4069(18) . ?
C4 C3 1.4038(17) . ?
C4 C12 1.4637(16) . ?
C5 N1 1.3527(16) . ?
C5 C6 1.4727(17) . ?
C12 N4 1.3290(16) . ?
C12 C11 1.4331(16) . ?
N4 C13 1.3609(15) . ?
N1 C1 1.3322(17) . ?
C7 C8 1.4012(17) . ?
C7 C6 1.4061(17) . ?
C7 C11 1.4605(17) . ?
N3 C11 1.3272(16) . ?
N3 C18 1.3532(16) . ?
C15 C14 1.3726(17) . ?
C15 C16 1.4320(16) . ?
C6 N2 1.3539(17) . ?
C14 C13 1.4217(17) . ?
C3 C2 1.3812(17) . ?
C16 C17 1.3622(18) . ?
C13 C18 1.4205(16) . ?
C10 N2 1.3258(17) . ?
C10 C9 1.3987(18) . ?
C18 C17 1.4206(16) . ?
C20 N6 1.1499(18) . ?
C8 C9 1.3764(18) . ?
C1 C2 1.3954(19) . ?
C19 N5 1.1524(18) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660989
