#------------------------------------------------------------------------------
#$Date: 2019-11-28 12:59:13 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243845 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/23/7702379.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_7702379
loop_
_publ_author_name
'Marder, Todd B.'
'Norman, Nicholas C.'
'Orpen, A. Guy'
'Quayle, Michael J.'
'Rice, Craig R.'
_publ_section_title
;
 Crystalline TCNQ and TCNE adducts of the diborane(4) compounds
 B2(1,2-E2C6H4)2 (E = O or S)
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2127
_journal_paper_doi               10.1039/a901169b
_journal_year                    1999
_chemical_formula_structural     'B S2 C6 H4 ^.^ TCNE'
_chemical_formula_sum            'C18 H8 B2 N4 S4'
_chemical_formula_weight         430.14
_chemical_name_systematic
; 
 tetracyanoethene - bis(Benzene-1,2-dithiolato)
-diborane adduct 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                80.80(2)
_cell_angle_beta                 79.61(3)
_cell_angle_gamma                64.00(2)
_cell_formula_units_Z            1
_cell_length_a                   6.861(3)
_cell_length_b                   7.172(3)
_cell_length_c                   10.862(3)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      5
_cell_volume                     470.5(3)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4889
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             218
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0197(54)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.967
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_obs          0.0470
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0668P)²+0.0000P] where P=(Max(Fo²,0)+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1211
_refine_ls_wR_factor_obs         0.1156
_reflns_number_observed          1523
_reflns_number_total             2123
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901169b.txt
_cod_data_source_block           6.2
_cod_depositor_comments
;
The following automatic conversions were performed:

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

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.0000P] where
P=(Max(Fo^2^,0)+2Fc^2^)/3' was changed to 'calc'. A new data item
'_refine_ls_weighting_details' was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.0000P] where
P=(Max(Fo^2^,0)+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702379
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
B1 0.028(2) 0.020(2) 0.018(2) 0.0003(12) -0.0011(13) -0.0133(14)
S1 0.0249(4) 0.0184(4) 0.0283(4) 0.0073(3) -0.0035(3) -0.0135(3)
S2 0.0241(4) 0.0196(4) 0.0246(4) 0.0053(3) -0.0035(3) -0.0098(3)
C1 0.026(2) 0.0172(13) 0.0172(13) 0.0028(10) -0.0011(11) -0.0137(12)
C2 0.0246(15) 0.0157(13) 0.0188(13) 0.0024(10) -0.0027(11) -0.0106(11)
C3 0.026(2) 0.027(2) 0.0227(14) 0.0001(12) 0.0006(12) -0.0188(13)
C4 0.040(2) 0.024(2) 0.0224(14) 0.0034(12) -0.0009(13) -0.0234(14)
C5 0.036(2) 0.0156(14) 0.0233(14) 0.0047(11) -0.0062(12) -0.0122(13)
C6 0.025(2) 0.0208(15) 0.0243(14) 0.0024(11) -0.0038(12) -0.0117(12)
C7 0.0269(15) 0.0233(15) 0.0185(13) 0.0023(11) -0.0024(11) -0.0157(13)
C8 0.0216(15) 0.026(2) 0.0242(14) 0.0027(12) -0.0018(12) -0.0135(13)
C9 0.024(2) 0.025(2) 0.0256(15) 0.0043(12) -0.0063(12) -0.0113(13)
N8 0.0296(14) 0.0287(15) 0.0332(14) 0.0059(12) -0.0033(11) -0.0161(12)
N9 0.034(2) 0.035(2) 0.0370(15) 0.0098(12) -0.0065(12) -0.0241(13)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
B1 B 0.5137(5) 0.3854(5) 0.0403(3) 0.0215(7) Uani 1 d .
S1 S 0.76867(12) 0.18956(11) 0.08499(7) 0.0234(2) Uani 1 d .
S2 S 0.29305(12) 0.31045(11) 0.08972(6) 0.0233(2) Uani 1 d .
C1 C 0.6712(5) 0.0043(4) 0.1569(2) 0.0191(6) Uani 1 d .
C2 C 0.4473(5) 0.0624(4) 0.1605(2) 0.0194(6) Uani 1 d .
C3 C 0.3562(5) -0.0751(4) 0.2170(2) 0.0233(6) Uani 1 d .
H3A H 0.2038(5) -0.0352(4) 0.2209(2) 0.028 Uiso 1 calc R
C4 C 0.4914(5) -0.2713(5) 0.2676(3) 0.0260(7) Uani 1 d .
H4A H 0.4308(5) -0.3662(5) 0.3056(3) 0.031 Uiso 1 calc R
C5 C 0.7149(5) -0.3301(4) 0.2633(3) 0.0251(6) Uani 1 d .
H5A H 0.8054(5) -0.4650(4) 0.2977(3) 0.030 Uiso 1 calc R
C6 C 0.8056(5) -0.1933(4) 0.2091(3) 0.0229(6) Uani 1 d .
H6A H 0.9575(5) -0.2328(4) 0.2074(3) 0.028 Uiso 1 calc R
C7 C 0.6095(5) -0.0437(4) 0.5017(2) 0.0216(6) Uani 1 d .
C8 C 0.7180(5) -0.2528(5) 0.5585(3) 0.0236(6) Uani 1 d .
C9 C 0.7353(5) 0.0724(5) 0.4498(3) 0.0248(6) Uani 1 d .
N8 N 0.7988(4) -0.4198(4) 0.6033(2) 0.0303(6) Uani 1 d .
N9 N 0.8334(4) 0.1669(4) 0.4080(2) 0.0331(6) Uani 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'
B B 0.0013 0.0007 '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
B1 B1 S2 123.9(3) 2_665 .
B1 B1 S1 123.4(3) 2_665 .
S2 B1 S1 112.8(2) . .
C1 S1 B1 96.92(15) . .
C1 S1 S1 92.56(10) . 2_755
B1 S1 S1 132.61(11) . 2_755
C2 S2 B1 96.80(14) . .
C2 C1 C6 120.1(3) . .
C2 C1 S1 116.6(2) . .
C6 C1 S1 123.3(2) . .
C3 C2 C1 120.2(3) . .
C3 C2 S2 122.9(2) . .
C1 C2 S2 116.9(2) . .
C4 C3 C2 119.2(3) . .
C3 C4 C5 120.7(3) . .
C6 C5 C4 120.4(3) . .
C5 C6 C1 119.4(3) . .
C7 C7 C9 120.2(3) 2_656 .
C7 C7 C8 120.5(3) 2_656 .
C9 C7 C8 119.3(3) . .
N8 C8 C7 178.0(3) . .
N9 C9 C7 179.2(3) . .
C8 N8 H4A 121.1(2) . 2_646
C9 N9 H5A 144.4(2) . 1_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 B1 1.682(6) 2_665
B1 S2 1.788(3) .
B1 S1 1.790(3) .
S1 C1 1.755(3) .
S1 S1 3.578(2) 2_755
S2 C2 1.755(3) .
C1 C2 1.399(4) .
C1 C6 1.402(4) .
C2 C3 1.396(4) .
C3 C4 1.391(4) .
C4 C5 1.394(4) .
C5 C6 1.384(4) .
C7 C7 1.356(6) 2_656
C7 C9 1.435(4) .
C7 C8 1.440(4) .
C8 N8 1.144(4) .
C9 N9 1.145(4) .
N8 H4A 2.624(4) 2_646
N9 H5A 2.658(4) 1_565
