# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_BiSCN3
_database_code_depnum_ccdc_archive 'CCDC 1860296'
#Added by publCIF



_audit_update_record             
;
2018-08-05 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_BiSCN3              
;
PROBLEM: Non-Solvent  Resd 1  S   Ueq(max)/Ueq(min) Range        3.1 Ratio
RESPONSE: This thiocyanate ligand is somewhat disordered, but this disorder  could not be resolved using a multi-site model, and so leads to large   and anisotropic ADPs.
;
_vrf_PLAT241_BiSCN3              
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       N00G Check
RESPONSE:  It is common for thiocyanate bound to heavy metals to show  significantly more thermal motion than the metal it is bound to.
;
_vrf_PLAT242_BiSCN3              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C00J Check
RESPONSE: This thiocyanate ligand is somewhat disordered, but this disorder  could not be resolved using a multi-site model, and so leads to large   and anisotropic ADPs on the S atom, compared to the adjacent C.
;
# Added during the CSD deposition process: Sunday 05 August 2018 01:39 PM
# end Validation Reply Form



_refine_ls_number_constraints    0
#Added by publCIF




_symmetry_space_group_name_hall  '-P 1'
# publcif _publ_body_element loop end
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            'bismuth(III) thiocyanate'
_chemical_formula_moiety         'C6 Bi2 N6 S6'
_chemical_formula_sum            'C6 Bi2 N6 S6'
_chemical_formula_weight         766.44
_chemical_melting_point          decomposes
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5960(2)
_cell_length_b                   11.7359(4)
_cell_length_c                   12.0300(4)
_cell_angle_alpha                114.088(2)
_cell_angle_beta                 102.485(2)
_cell_angle_gamma                98.3880(10)
_cell_volume                     800.90(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1949
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_temperature    180(2)
_diffrn_measurement_method       CCD

_exptl_absorpt_coefficient_mu    22.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_T_max  1.0
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.178
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5145
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.947
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device       KappaCCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2911
_reflns_number_total             3518
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.597
_refine_diff_density_min         -3.165
_refine_diff_density_rms         0.363
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3518
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0425
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0520P)²+7.8601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1109

_atom_sites_solution_primary     dual

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi01 Bi 0.62100(6) 0.43379(4) 0.73133(3) 0.01716(13) Uani 1 1 d . . . . .
Bi02 Bi 0.48119(6) -0.08418(4) 0.21280(3) 0.01766(13) Uani 1 1 d . . . . .
S003 S 0.1676(5) 0.3663(3) 0.2892(3) 0.0312(7) Uani 1 1 d . . . A 1
S004 S 0.2591(4) 0.1675(3) 0.6103(2) 0.0215(5) Uani 1 1 d . . . . .
S005 S 0.3246(5) 0.5539(3) 0.8096(3) 0.0272(6) Uani 1 1 d . . . . .
S006 S 0.8099(5) 0.1286(3) 0.3056(3) 0.0338(7) Uani 1 1 d . . . . .
S007 S 1.0717(4) 0.7460(3) 1.2022(2) 0.0243(6) Uani 1 1 d . . . . .
S008 S 0.7975(7) -0.0294(6) -0.1295(5) 0.0654(14) Uani 1 1 d . . . B 1
N009 N 0.4609(16) 0.6481(9) 1.0771(9) 0.026(2) Uani 1 1 d . . . . .
N00A N 0.3714(16) 0.0277(9) 0.3911(8) 0.026(2) Uani 1 1 d . . . . .
C00B C 0.3270(17) 0.0852(10) 0.4814(9) 0.017(2) Uani 1 1 d . . . . .
N00C N 0.8747(14) 0.5882(9) 0.9386(8) 0.0219(19) Uani 1 1 d . . . . .
N00D N 0.6160(18) -0.1043(10) 0.0279(9) 0.030(2) Uani 1 1 d . . . . .
C00E C 0.2796(18) 0.3964(11) 0.4395(10) 0.024(2) Uani 1 1 d . . . A 1
N00F N 0.3521(16) 0.4136(10) 0.5425(9) 0.026(2) Uani 1 1 d . . . . .
N00G N 0.7469(18) 0.2968(11) 0.5316(10) 0.038(3) Uani 1 1 d . . . . .
C00H C 0.4062(17) 0.6068(11) 0.9662(10) 0.022(2) Uani 1 1 d . . . . .
C00I C 0.770(2) 0.2263(12) 0.4396(11) 0.029(3) Uani 1 1 d . . . . .
C00J C 0.684(2) -0.0734(12) -0.0394(10) 0.028(3) Uani 1 1 d . . . . .
C00K C 0.9591(17) 0.6542(11) 1.0477(9) 0.020(2) Uani 1 1 d . . . . .

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
Bi01 0.0174(2) 0.0194(2) 0.0124(2) 0.00607(16) 0.00305(15) 0.00396(16)
Bi02 0.0202(2) 0.0182(2) 0.0127(2) 0.00568(16) 0.00574(15) 0.00269(16)
S003 0.0305(16) 0.0339(16) 0.0201(14) 0.0160(12) -0.0059(12) -0.0083(13)
S004 0.0226(14) 0.0251(14) 0.0170(12) 0.0081(10) 0.0087(10) 0.0079(11)
S005 0.0234(14) 0.0394(17) 0.0196(13) 0.0126(12) 0.0060(11) 0.0144(13)
S006 0.0324(17) 0.0259(15) 0.0300(16) 0.0008(12) 0.0179(13) -0.0060(13)
S007 0.0182(13) 0.0313(15) 0.0139(13) 0.0033(11) 0.0051(10) -0.0002(11)
S008 0.051(2) 0.138(4) 0.084(3) 0.097(3) 0.049(2) 0.060(3)
N009 0.028(5) 0.022(5) 0.024(5) 0.006(4) 0.012(4) 0.006(4)
N00A 0.026(5) 0.030(5) 0.015(5) 0.005(4) 0.008(4) 0.003(4)
C00B 0.022(5) 0.017(5) 0.010(5) 0.005(4) 0.001(4) 0.005(4)
N00C 0.015(5) 0.029(5) 0.020(5) 0.012(4) 0.005(4) 0.001(4)
N00D 0.043(6) 0.035(6) 0.031(5) 0.023(5) 0.023(5) 0.020(5)
C00E 0.023(6) 0.027(6) 0.023(6) 0.015(5) 0.006(5) 0.007(5)
N00F 0.025(5) 0.035(6) 0.019(5) 0.017(4) 0.003(4) 0.003(4)
N00G 0.035(6) 0.031(6) 0.030(6) 0.000(5) 0.005(5) 0.001(5)
C00H 0.016(5) 0.026(6) 0.015(5) 0.003(4) 0.003(4) 0.004(4)
C00I 0.026(6) 0.035(7) 0.026(6) 0.014(5) 0.010(5) 0.006(5)
C00J 0.035(7) 0.040(7) 0.019(5) 0.019(5) 0.011(5) 0.022(6)
C00K 0.014(5) 0.029(6) 0.015(5) 0.008(4) 0.006(4) 0.008(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Bi01 S003 2.679(3) 2_666 ?
Bi01 S005 2.686(3) . ?
Bi01 N00C 2.434(9) . ?
Bi01 N00F 2.462(9) . ?
Bi01 N00G 2.674(11) . ?
Bi02 S004 3.005(3) 2_656 ?
Bi02 S006 2.699(3) . ?
Bi02 S007 3.059(3) 1_444 ?
Bi02 S008 2.677(3) 2_655 ?
Bi02 N00A 2.345(9) . ?
Bi02 N00D 2.506(9) . ?
S003 Bi01 2.679(3) 2_666 ?
S003 C00E 1.663(11) . ?
S004 Bi02 3.005(3) 2_656 ?
S004 C00B 1.656(10) . ?
S005 C00H 1.654(10) . ?
S006 C00I 1.658(12) . ?
S007 Bi02 3.059(3) 1_666 ?
S007 C00K 1.644(10) . ?
S008 Bi02 2.677(3) 2_655 ?
S008 C00J 1.642(12) . ?
N009 C00H 1.165(14) . ?
N00A C00B 1.148(13) . ?
N00C C00K 1.167(13) . ?
N00D C00J 1.157(15) . ?
C00E N00F 1.147(14) . ?
N00G C00I 1.136(15) . ?

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
S003 Bi01 S005 93.31(10) 2_666 . ?
N00C Bi01 S003 70.7(2) . 2_666 ?
N00C Bi01 S005 86.6(2) . . ?
N00C Bi01 N00F 143.8(3) . . ?
N00C Bi01 N00G 122.6(3) . . ?
N00F Bi01 S003 81.9(2) . 2_666 ?
N00F Bi01 S005 71.6(2) . . ?
N00F Bi01 N00G 74.6(3) . . ?
N00G Bi01 S003 82.5(3) . 2_666 ?
N00G Bi01 S005 146.2(3) . . ?
S004 Bi02 S007 89.16(8) 2_656 1_444 ?
S006 Bi02 S004 88.59(10) . 2_656 ?
S006 Bi02 S007 157.25(8) . 1_444 ?
S008 Bi02 S004 159.19(10) 2_655 2_656 ?
S008 Bi02 S006 91.59(14) 2_655 . ?
S008 Bi02 S007 82.68(12) 2_655 1_444 ?
N00A Bi02 S004 83.0(2) . 2_656 ?
N00A Bi02 S006 87.0(3) . . ?
N00A Bi02 S007 70.3(3) . 1_444 ?
N00A Bi02 S008 76.3(3) . 2_655 ?
N00A Bi02 N00D 154.0(3) . . ?
N00D Bi02 S004 114.0(2) . 2_656 ?
N00D Bi02 S006 74.5(3) . . ?
N00D Bi02 S007 126.7(3) . 1_444 ?
N00D Bi02 S008 86.0(2) . 2_655 ?
C00E S003 Bi01 104.5(4) . 2_666 ?
C00B S004 Bi02 98.0(3) . 2_656 ?
C00H S005 Bi01 103.4(4) . . ?
C00I S006 Bi02 102.4(5) . . ?
C00K S007 Bi02 102.3(4) . 1_666 ?
C00J S008 Bi02 102.1(4) . 2_655 ?
C00B N00A Bi02 177.0(9) . . ?
N00A C00B S004 179.1(10) . . ?
C00K N00C Bi01 164.6(8) . . ?
C00J N00D Bi02 158.9(9) . . ?
N00F C00E S003 177.8(12) . . ?
C00E N00F Bi01 158.4(9) . . ?
C00I N00G Bi01 169.5(10) . . ?
N009 C00H S005 177.5(10) . . ?
N00G C00I S006 177.6(13) . . ?
N00D C00J S008 175.9(11) . . ?
N00C C00K S007 178.4(10) . . ?





_iucr_refine_instructions_details 
;

    import.res created by SHELXL-2014/7

TITL import_a.res in P-1
REM Old TITL GLOBAL OLEX2: imported from CIF
REM SHELXT solution in P-1
REM R1 0.079, Rweak 0.004, Alpha 0.067, Orientation as input
REM Formula found by SHELXT: Bi2 S6 C6 N5 O
CELL 0.71073 6.596 11.7359 12.03 114.088 102.485 98.388
ZERR 4 0.0002 0.0004 0.0004 0.002 0.002 0.001
LATT 1
SFAC Bi C N S
UNIT 4 12 12 12
 
L.S. 4
PLAN  20
BOND $H
list 4
fmap 2
acta
OMIT 0 -1 1
OMIT 0 1 1
REM <olex2.extras>
REM <HklSrc "%./import.hkl">
REM </olex2.extras>
 
WGHT    0.052000    7.860100
FVAR       0.34534
BI01  1    0.621001    0.433790    0.731331    11.00000    0.01743    0.01937 =
         0.01236    0.00607    0.00305    0.00396
BI02  1    0.481187   -0.084177    0.212805    11.00000    0.02020    0.01824 =
         0.01265    0.00568    0.00574    0.00269
PART 1
S003  4    0.167629    0.366279    0.289207    11.00000    0.03054    0.03391 =
         0.02010    0.01599   -0.00590   -0.00828
PART 0
S004  4    0.259110    0.167490    0.610317    11.00000    0.02262    0.02510 =
         0.01702    0.00805    0.00874    0.00786
S005  4    0.324579    0.553919    0.809581    11.00000    0.02343    0.03942 =
         0.01957    0.01257    0.00600    0.01443
S006  4    0.809915    0.128609    0.305590    11.00000    0.03244    0.02586 =
         0.02995    0.00083    0.01791   -0.00599
S007  4    1.071687    0.745954    1.202230    11.00000    0.01815    0.03132 =
         0.01388    0.00329    0.00513   -0.00019
PART 1
S008  4    0.797507   -0.029404   -0.129515    11.00000    0.05068    0.13845 =
         0.08404    0.09733    0.04863    0.05968
PART 0
N009  3    0.460873    0.648054    1.077095    11.00000    0.02768    0.02207 =
         0.02390    0.00586    0.01187    0.00568
N00A  3    0.371443    0.027675    0.391078    11.00000    0.02622    0.02995 =
         0.01529    0.00462    0.00788    0.00297
C00B  2    0.327012    0.085199    0.481379    11.00000    0.02192    0.01663 =
         0.01043    0.00486    0.00128    0.00515
N00C  3    0.874723    0.588165    0.938601    11.00000    0.01545    0.02925 =
         0.01968    0.01159    0.00501    0.00086
N00D  3    0.615983   -0.104303    0.027896    11.00000    0.04288    0.03505 =
         0.03090    0.02320    0.02259    0.02040
PART 1
C00E  2    0.279560    0.396391    0.439546    11.00000    0.02316    0.02716 =
         0.02337    0.01486    0.00597    0.00713
PART 0
N00F  3    0.352070    0.413622    0.542487    11.00000    0.02520    0.03525 =
         0.01926    0.01677    0.00282    0.00292
N00G  3    0.746918    0.296802    0.531563    11.00000    0.03458    0.03093 =
         0.03031    0.00027    0.00547    0.00123
C00H  2    0.406203    0.606819    0.966238    11.00000    0.01640    0.02570 =
         0.01509    0.00300    0.00343    0.00431
C00I  2    0.769557    0.226329    0.439575    11.00000    0.02591    0.03541 =
         0.02560    0.01375    0.01028    0.00627
C00J  2    0.684022   -0.073374   -0.039405    11.00000    0.03514    0.04044 =
         0.01879    0.01881    0.01064    0.02215
C00K  2    0.959132    0.654212    1.047708    11.00000    0.01442    0.02935 =
         0.01518    0.00768    0.00606    0.00792
HKLF 4
 
REM  import_a.res in P-1
REM R1 =  0.0425 for    2911 Fo > 4sig(Fo)  and  0.0550 for all    3518 data
REM    181 parameters refined using      0 restraints
 
END  
     
WGHT      0.0520      7.8600 

REM Highest difference peak  2.597,  deepest hole -3.165,  1-sigma level  0.363
Q1    1   0.4903 -0.1749  0.2184  11.00000  0.05    2.60
Q2    1   0.6152  0.5145  0.7278  11.00000  0.05    2.39
Q3    1   0.6281  0.3493  0.7316  11.00000  0.05    2.30
Q4    1   0.4866  0.0116  0.2241  11.00000  0.05    2.17
Q5    1   0.7939  0.4628  0.7071  11.00000  0.05    1.74
Q6    1   0.2997 -0.1195  0.2238  11.00000  0.05    1.71
Q7    1   0.8044  0.0472  0.2989  11.00000  0.05    1.39
Q8    1   0.5317  0.5803  0.7185  11.00000  0.05    1.35
Q9    1   0.4193  0.2396  0.7581  11.00000  0.05    1.30
Q10   1   0.4117  0.7338  0.8403  11.00000  0.05    1.28
Q11   1   0.5277  0.0277  0.1376  11.00000  0.05    1.27
Q12   1   0.6404 -0.0457  0.1841  11.00000  0.05    1.26
Q13   1   0.6544  0.3547  0.6599  11.00000  0.05    1.23
Q14   1   0.4385  0.3971  0.7470  11.00000  0.05    1.19
Q15   1   1.2865  0.7210  1.2378  11.00000  0.05    1.18
Q16   1   0.7607 -0.0458  0.2451  11.00000  0.05    1.16
Q17   1   0.6718  0.0173  0.4205  11.00000  0.05    1.15
Q18   1   0.4133  0.0824  0.6198  11.00000  0.05    1.15
Q19   1   0.9421  0.2009  0.4182  11.00000  0.05    1.10
Q20   1   0.5562 -0.1485  0.1586  11.00000  0.05    1.09

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0425 for 2911 Fo > 4sig(Fo) and 0.0550 for all 5149 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.60, deepest hole -3.16
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0550
  REM R1_gt = 0.0425
  REM wR_ref = 0.1109
  REM GOOF = 1.040
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 5149
  REM Reflections_gt = 2911
  REM Parameters = n/a
  REM Hole = -3.16
  REM Peak = 2.60
  REM Flack = n/a

  
;

#==============================================================================
# start Validation Reply Forms
#==============================================================================
_vrf_PLAT971_ALERT_2_B           
;
PROBLEM: Check Calcd Resid. Dens.  1.04A   From Bi02            2.82 eA-3 
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples. The size of the positive and negative ripples are
 less than 4% of the number of electrons on the heaviest atom (Bi) and 
 approximately equal. The low symmetry of the structure means the multi-scan
 absorption correction may not be optimal.
;

_vrf_PLAT972_ALERT_2_B           
;
PROBLEM: Check Calcd Resid. Dens.  0.66A   From Bi02           -3.14 eA-3 
		 Check Calcd Resid. Dens.  0.75A   From Bi01           -2.62 eA-3
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples. The size of the positive and negative ripples are
 less than 4% of the number of electrons on the heaviest atom (Bi) and 
 approximately equal. The low symmetry of the structure means the multi-scan
 absorption correction may not be optimal.
;

_vrf_PLAT971_ALERT_2_C           
;
PROBLEM: Check Calcd Resid. Dens.  1.04A   From Bi01            2.47 eA-3  
		 Check Calcd Resid. Dens.  1.06A   From Bi02            2.37 eA-3  
		 Check Calcd Resid. Dens.  0.85A   From Bi01            2.30 eA-3  
		 Check Calcd Resid. Dens.  1.30A   From Bi01            1.96 eA-3  
		 Check Calcd Resid. Dens.  1.24A   From Bi02            1.70 eA-3  
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples. The size of the positive and negative ripples are
 less than 4% of the number of electrons on the heaviest atom (Bi) and 
 approximately equal. The low symmetry of the structure means the multi-scan
 absorption correction may not be optimal.	 
;
_vrf_PLAT972_ALERT_2_C           
;
PROBLEM: Check Calcd Resid. Dens.  0.80A   From Bi01           -2.47 eA-3  
		 Check Calcd Resid. Dens.  0.71A   From Bi01           -2.38 eA-3  
		 Check Calcd Resid. Dens.  0.70A   From Bi02           -2.29 eA-3  
		 Check Calcd Resid. Dens.  0.81A   From Bi02           -2.15 eA-3  
		 Check Calcd Resid. Dens.  0.70A   From Bi02           -2.14 eA-3  
		 Check Calcd Resid. Dens.  0.84A   From Bi01           -2.12 eA-3  
		 Check Calcd Resid. Dens.  1.04A   From Bi01           -2.10 eA-3  
		 Check Calcd Resid. Dens.  0.86A   From Bi01           -2.09 eA-3  
		 Check Calcd Resid. Dens.  0.80A   From Bi02           -1.97 eA-3  
		 Check Calcd Resid. Dens.  1.43A   From Bi02           -1.80 eA-3  
		 Check Calcd Resid. Dens.  1.30A   From Bi01           -1.58 eA-3   
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples. The size of the positive and negative ripples are
 less than 4% of the number of electrons on the heaviest atom (Bi) and 
 approximately equal. The low symmetry of the structure means the multi-scan
 absorption correction may not be optimal.	 
;
#==============================================================================
#==============================================================================

_vrf_PLAT220_ALERT_2_C           
;
PROBLEM: Non-Solvent  Resd 1  S   Ueq(max)/Ueq(min) Range        3.1 Ratio 
RESPONSE: This thiocyanate ligand is somewhat disordered, but this disorder
 could not be resolved using a multi-site model, and so leads to large 
 and anisotropic ADPs.
;

_vrf_PLAT242_ALERT_2_C           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       C00J Check 
RESPONSE: This thiocyanate ligand is somewhat disordered, but this disorder
 could not be resolved using a multi-site model, and so leads to large 
 and anisotropic ADPs on the S atom, compared to the adjacent C.
;

_vrf_PLAT241_ALERT_2_C           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       N00G Check 
RESPONSE: It is common for thiocyanate bound to heavy metals to show 
significantly more thermal motion than the metal it is bound to.
;

#==============================================================================
#==============================================================================

_vrf_PLAT911_ALERT_3_C           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         19 Report
RESPONSE: A small number of low angle reflections are missing due to the 
low symmetry of the structure, beam stop and the data collection strategy.
;



_publcif_funding_html            
;
;
_chemical_name_systematic        'bismuth(III) thiocyanate'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FeBiSCN6_180K
_database_code_depnum_ccdc_archive 'CCDC 1860297'
_audit_update_record             
;
2018-08-05 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT241_FeBiSCN6_180K       
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S5 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_FeBiSCN6_180K       
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Bi1 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
# Added during the CSD deposition process: Sunday 05 August 2018 01:39 PM
# end Validation Reply Form

_audit_creation_date             2018-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'iron(III) hexathiocyanatobismuthate'
_chemical_formula_moiety         '0.5(Bi2 C12 Fe2 N12 S12)'
_chemical_formula_sum            'C6 Bi Fe N6 S6'
_chemical_formula_weight         613.31
_chemical_melting_point          decomposes
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.39280(10)
_cell_length_b                   8.45120(10)
_cell_length_c                   12.0977(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.2440(10)
_cell_angle_gamma                90
_cell_volume                     858.07(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21914
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_temperature    180
_diffrn_measurement_method       CCD
_exptl_absorpt_coefficient_mu    11.810
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'

_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.374

_exptl_crystal_description       block
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3672
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         3.818
_diffrn_ambient_temperature      180
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'

_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1730
_reflns_number_total             1929
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.611
_refine_diff_density_min         -1.615
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1929
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0234
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+1.8124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0596

_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 1.0000 1.0000 0.5000 0.01817(8) Uani 1 2 d S T P . .
Fe2 Fe 0.5000 0.5000 0.5000 0.01703(17) Uani 1 2 d S T P . .
S3 S 1.02037(12) 0.69823(13) 0.40175(10) 0.0338(3) Uani 1 1 d . . . . .
S4 S 1.25124(16) 0.96495(16) 0.65375(10) 0.0386(3) Uani 1 1 d . . . . .
S5 S 1.24895(14) 1.0822(2) 0.35629(9) 0.0467(4) Uani 1 1 d . . . . .
N6 N 0.4085(4) 0.7123(4) 0.5524(3) 0.0267(7) Uani 1 1 d . . . . .
C7 C 0.8371(4) 0.6431(5) 0.4328(3) 0.0223(8) Uani 1 1 d . . . . .
N8 N 0.4082(4) 0.5369(5) 0.3455(3) 0.0260(7) Uani 1 1 d . . . . .
N9 N 0.7109(4) 0.6037(4) 0.4541(3) 0.0247(7) Uani 1 1 d . . . . .
C10 C 1.1545(5) 1.0542(5) 0.2390(3) 0.0243(8) Uani 1 1 d . . . . .
C1 C 0.3426(4) 0.8173(5) 0.5933(3) 0.0247(8) Uani 1 1 d . . . . .

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
Bi1 0.01472(12) 0.02303(13) 0.01677(12) -0.00211(7) 0.00066(8) -0.00069(7)
Fe2 0.0130(4) 0.0219(4) 0.0162(4) -0.0010(3) -0.0005(3) 0.0006(2)
S3 0.0180(4) 0.0294(5) 0.0542(7) -0.0091(5) 0.0120(4) -0.0028(4)
S4 0.0444(7) 0.0431(6) 0.0284(6) -0.0131(5) -0.0100(5) 0.0230(5)
S5 0.0306(6) 0.0899(11) 0.0197(5) -0.0051(6) -0.0015(4) -0.0294(6)
N6 0.0214(16) 0.0287(18) 0.0299(17) -0.0055(14) -0.0020(13) 0.0011(13)
C7 0.0218(19) 0.0225(19) 0.0226(18) -0.0013(15) 0.0010(15) 0.0031(15)
N8 0.0227(17) 0.0365(19) 0.0187(17) 0.0004(14) 0.0005(14) 0.0040(14)
N9 0.0181(15) 0.0286(18) 0.0274(17) 0.0001(14) 0.0021(13) -0.0032(13)
C10 0.0204(19) 0.030(2) 0.023(2) 0.0002(17) 0.0032(15) -0.0091(16)
C1 0.0206(18) 0.030(2) 0.0239(19) -0.0013(16) -0.0057(15) 0.0045(15)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Bi1 S3 2.8192(11) . ?
Bi1 S3 2.8192(11) 3_776 ?
Bi1 S4 2.8214(12) . ?
Bi1 S4 2.8214(12) 3_776 ?
Bi1 S5 2.8108(11) 3_776 ?
Bi1 S5 2.8109(11) . ?
Fe2 N6 2.053(3) 3_666 ?
Fe2 N6 2.053(3) . ?
Fe2 N8 2.043(3) 3_666 ?
Fe2 N8 2.043(3) . ?
Fe2 N9 2.053(3) 3_666 ?
Fe2 N9 2.053(3) . ?
S3 C7 1.652(4) . ?
S4 C1 1.638(4) 1_655 ?
S5 C10 1.640(4) . ?
N6 C1 1.158(5) . ?
C7 N9 1.141(5) . ?
N8 C10 1.156(5) 2_645 ?
C10 N8 1.156(5) 2_655 ?
C1 S4 1.638(4) 1_455 ?

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
S3 Bi1 S3 180.000(19) . 3_776 ?
S3 Bi1 S4 82.15(3) 3_776 . ?
S3 Bi1 S4 82.16(3) . 3_776 ?
S3 Bi1 S4 97.84(3) 3_776 3_776 ?
S3 Bi1 S4 97.85(3) . . ?
S4 Bi1 S4 180.0 . 3_776 ?
S5 Bi1 S3 94.81(4) 3_776 . ?
S5 Bi1 S3 94.81(4) . 3_776 ?
S5 Bi1 S3 85.19(4) . . ?
S5 Bi1 S3 85.19(4) 3_776 3_776 ?
S5 Bi1 S4 96.99(4) 3_776 . ?
S5 Bi1 S4 83.01(4) 3_776 3_776 ?
S5 Bi1 S4 83.01(4) . . ?
S5 Bi1 S4 96.99(4) . 3_776 ?
S5 Bi1 S5 180.0 3_776 . ?
N6 Fe2 N6 180.0 3_666 . ?
N8 Fe2 N6 90.53(14) . . ?
N8 Fe2 N6 89.47(14) . 3_666 ?
N8 Fe2 N6 90.53(14) 3_666 3_666 ?
N8 Fe2 N6 89.47(14) 3_666 . ?
N8 Fe2 N8 180.00(18) 3_666 . ?
N8 Fe2 N9 89.44(14) . 3_666 ?
N8 Fe2 N9 90.56(14) 3_666 3_666 ?
N8 Fe2 N9 89.44(14) 3_666 . ?
N8 Fe2 N9 90.56(14) . . ?
N9 Fe2 N6 88.03(13) 3_666 . ?
N9 Fe2 N6 91.97(13) 3_666 3_666 ?
N9 Fe2 N6 88.03(13) . 3_666 ?
N9 Fe2 N6 91.97(13) . . ?
N9 Fe2 N9 180.0 3_666 . ?
C7 S3 Bi1 95.80(14) . . ?
C1 S4 Bi1 97.79(13) 1_655 . ?
C10 S5 Bi1 98.15(14) . . ?
C1 N6 Fe2 169.0(3) . . ?
N9 C7 S3 179.4(4) . . ?
C10 N8 Fe2 175.0(3) 2_645 . ?
C7 N9 Fe2 171.0(3) . . ?
N8 C10 S5 177.8(4) 2_655 . ?
N6 C1 S4 178.7(4) . 1_455 ?

_iucr_refine_instructions_details 
;

    import-090118.res created by SHELXL-2014/7

TITL import-090118 in P21/n #14
REM reset to P21/n #14
CELL 0.71073 8.3928 8.4512 12.0977 90 90.244 90
ZERR 2 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Bi C Fe N S
UNIT 2 12 2 12 12
 
L.S. 4
PLAN  20
TEMP -93.15
BOND
fmap 2
acta
OMIT -1 1 1
OMIT 0 1 1
OMIT -1 0 1
OMIT -1 1 0
OMIT 1 0 1
OMIT 1 1 0
OMIT 0 0 2
REM <olex2.extras>
REM <HklSrc "%./import-090118.hkl">
REM </olex2.extras>
 
WGHT    0.025600    1.812400
FVAR       0.47692
BI1   1    1.000000    0.500000    0.500000    10.50000    0.01472    0.02303 =
         0.01677   -0.00211    0.00066   -0.00069
FE2   3    0.500000    0.000000    0.500000    10.50000    0.01297    0.02192 =
         0.01620   -0.00101   -0.00045    0.00056
S3    5    1.020369    0.198229    0.401747    11.00000    0.01799    0.02935 =
         0.05422   -0.00908    0.01198   -0.00283
S4    5    1.251242    0.464952    0.653751    11.00000    0.04435    0.04308 =
         0.02842   -0.01313   -0.01002    0.02296
S5    5    1.248948    0.582155    0.356291    11.00000    0.03061    0.08990 =
         0.01966   -0.00508   -0.00148   -0.02937
N6    4    0.408532    0.212336    0.552444    11.00000    0.02137    0.02871 =
         0.02991   -0.00553   -0.00202    0.00114
C7    2    0.837065    0.143062    0.432831    11.00000    0.02178    0.02246 =
         0.02261   -0.00130    0.00097    0.00311
N8    4    0.408198    0.036922    0.345478    11.00000    0.02272    0.03649 =
         0.01871    0.00036    0.00052    0.00397
N9    4    0.710870    0.103671    0.454147    11.00000    0.01806    0.02859 =
         0.02743    0.00014    0.00209   -0.00320
C10   2    1.154478    0.554239    0.238975    11.00000    0.02042    0.02980 =
         0.02256    0.00022    0.00318   -0.00912
C1    2    0.342590    0.317331    0.593296    11.00000    0.02061    0.02954 =
         0.02390   -0.00128   -0.00567    0.00453
HKLF 4
 
REM  import-090118 in P21/n #14
REM R1 =  0.0234 for    1730 Fo > 4sig(Fo)  and  0.0270 for all    1929 data
REM     94 parameters refined using      0 restraints
 
END  
     
WGHT      0.0255      1.8111 

REM Highest difference peak  0.611,  deepest hole -1.615,  1-sigma level  0.187
Q1    1   1.1468  0.4853  0.5570  11.00000  0.05    0.61
Q2    1   1.1021  0.3741  0.5429  11.00000  0.05    0.56
Q3    1   1.1204  0.5994  0.5483  11.00000  0.05    0.55
Q4    1   1.1222  0.3579  0.6222  11.00000  0.05    0.52
Q5    1   1.1279  0.4275  0.5662  11.00000  0.05    0.50
Q6    1   1.0450  0.2617  0.6630  11.00000  0.05    0.48
Q7    1   1.3001  0.4936  0.3323  11.00000  0.05    0.45
Q8    1   0.8962  0.2921  0.3268  11.00000  0.05    0.44
Q9    1   1.1967  0.3873  0.5783  11.00000  0.05    0.43
Q10   1   1.2509  0.5149  0.5597  11.00000  0.05    0.43
Q11   1   0.8748  0.3272  0.4021  11.00000  0.05    0.43
Q12   1   1.1729  0.6781  0.3350  11.00000  0.05    0.39
Q13   1   1.1157  0.4896  0.3258  11.00000  0.05    0.39
Q14   1   1.1058  0.6432  0.4880  11.00000  0.05    0.39
Q15   1   0.3623  0.0948  0.4379  11.00000  0.05    0.38
Q16   1   1.1853  0.6083  0.6064  11.00000  0.05    0.38
Q17   1   0.1744  0.3132  0.5503  11.00000  0.05    0.38
Q18   1   1.1524  0.5044  0.4347  11.00000  0.05    0.37
Q19   1   0.8076  0.3410  0.4566  11.00000  0.05    0.37
Q20   1   1.1544  0.2466  0.4872  11.00000  0.05    0.36

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0234 for 1730 Fo > 4sig(Fo) and 0.0270 for all 3818 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.61, deepest hole -1.62
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0270
  REM R1_gt = 0.0234
  REM wR_ref = 0.0596
  REM GOOF = 1.172
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3818
  REM Reflections_gt = 1730
  REM Parameters = n/a
  REM Hole = -1.62
  REM Peak = 0.61
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'




#==============================================================================
# start Validation Reply Forms
#==============================================================================
_vrf_PLAT241_ALERT_2_C           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S5 Check 
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_ALERT_2_C           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Bi1 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
#==============================================================================
#==============================================================================
_vrf_PLAT906_ALERT_3_C           
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.354 Check
RESPONSE: The most common place for a high value of K is in the lowest-
intensity bin in the table. Almost all area detector integration programs end 
up slightly underestimating the background, resulting in overestimated values 
of Fo, thus the high value of Fo/Fc. This is most obvious in the weakest 
intensities, since the small addition to Fo becomes insignificant in the ratio 
when Fo is large.
;
#==============================================================================
#==============================================================================
_vrf_PLAT911_ALERT_3_C           
;
PROLBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          6 Report
RESPONSE: Low angle reflections obscured by beam stop
;
#==============================================================================
#==============================================================================
_vrf_PLAT972_ALERT_2_C           
;
PROBLEM: Check Calcd Resid. Dens.  0.87A   From Bi1            -1.59 eA-3  
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples. These are a small fraction of the total number of
 electrons.
;
_vrf_PLAT974_ALERT_2_C           
;
PROBLEM: Check Calcd Negative Resid. Density on       Bi1      -1.19 eA-3  
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples. These are a small fraction of the total number of
 electrons.
;
#==============================================================================
#==============================================================================
# end Validation Reply Forms
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: butanone, THF'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FeBiSCN6_300K
_database_code_depnum_ccdc_archive 'CCDC 1860300'
_audit_update_record             
;
2018-08-05 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT241_FeBiSCN6_300K       
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S2 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_FeBiSCN6_300K       
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
# Added during the CSD deposition process: Sunday 05 August 2018 01:39 PM
# end Validation Reply Form

_audit_creation_date             2018-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'iron(III) hexathiocyanatobismuthate'
_chemical_formula_moiety         '0.5(Bi2 C12 Fe2 N12 S12)'
_chemical_formula_sum            'C6 Bi Fe N6 S6'
_chemical_formula_weight         613.31
_chemical_melting_point          decomposes
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.38400(10)
_cell_length_b                   8.49260(10)
_cell_length_c                   12.1272(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.0600(10)
_cell_angle_gamma                90
_cell_volume                     863.48(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2094
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_diffrn_measurement_method       CCD

_exptl_absorpt_coefficient_mu    11.736
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             566

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16

_diffrn_reflns_av_R_equivalents  0.0122
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3782
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         3.360
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD plate'

_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'

_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1754
_reflns_number_total             1969
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.635
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.234
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0297P)²+1.7376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0690

_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.0000 1.0000 0.5000 0.02834(9) Uani 1 2 d S T P . .
Fe1 Fe 0.5000 0.5000 0.5000 0.02674(19) Uani 1 2 d S T P . .
S3 S 1.01886(15) 0.69983(16) 0.40148(14) 0.0523(4) Uani 1 1 d . . . . .
S2 S 0.2530(2) 0.9642(2) 0.65162(13) 0.0589(4) Uani 1 1 d . . . . .
S1 S 0.74757(18) 0.4184(3) 0.85472(11) 0.0706(6) Uani 1 1 d . . . . .
N2 N 0.4081(5) 0.7118(5) 0.5522(3) 0.0402(9) Uani 1 1 d . . . . .
N3 N 0.7107(4) 0.6040(5) 0.4548(3) 0.0375(9) Uani 1 1 d . . . . .
N1 N 0.5906(5) 0.4631(6) 0.6547(4) 0.0411(10) Uani 1 1 d . . . . .
C3 C 0.8366(5) 0.6440(5) 0.4334(4) 0.0340(9) Uani 1 1 d . . . . .
C2 C 0.3427(5) 0.8166(6) 0.5924(4) 0.0360(10) Uani 1 1 d . . . . .
C1 C 0.6529(6) 0.4453(7) 0.7379(4) 0.0382(10) Uani 1 1 d . . . . .

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
Bi1 0.02473(13) 0.03502(15) 0.02527(14) -0.00145(9) 0.00057(8) -0.00088(8)
Fe1 0.0216(4) 0.0335(5) 0.0252(4) -0.0013(3) -0.0013(3) 0.0006(3)
S3 0.0293(6) 0.0448(7) 0.0829(10) -0.0152(7) 0.0179(6) -0.0045(5)
S2 0.0655(10) 0.0657(9) 0.0455(8) -0.0209(7) -0.0171(7) 0.0328(8)
S1 0.0471(8) 0.1362(17) 0.0286(6) 0.0077(8) -0.0014(5) 0.0448(10)
N2 0.035(2) 0.039(2) 0.047(2) -0.0084(18) -0.0041(17) 0.0051(17)
N3 0.0275(19) 0.040(2) 0.045(2) -0.0013(18) 0.0021(16) -0.0042(16)
N1 0.036(2) 0.057(3) 0.031(2) 0.0009(19) -0.0011(17) 0.0058(19)
C3 0.034(2) 0.033(2) 0.035(2) -0.0034(19) 0.0019(17) 0.0019(19)
C2 0.031(2) 0.041(3) 0.036(2) -0.001(2) -0.0071(18) 0.0040(19)
C1 0.033(2) 0.050(3) 0.032(2) 0.000(2) 0.0032(18) 0.011(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Bi1 S3 2.8198(14) 1_455 ?
Bi1 S3 2.8198(14) 3_676 ?
Bi1 S2 2.8225(15) 3_576 ?
Bi1 S2 2.8225(15) . ?
Bi1 S1 2.8108(14) 2_556 ?
Bi1 S1 2.8108(14) 4_575 ?
Fe1 N2 2.057(4) . ?
Fe1 N2 2.057(4) 3_666 ?
Fe1 N3 2.050(4) 3_666 ?
Fe1 N3 2.050(4) . ?
Fe1 N1 2.047(4) 3_666 ?
Fe1 N1 2.047(4) . ?
S3 Bi1 2.8198(14) 1_655 ?
S3 C3 1.646(5) . ?
S2 C2 1.628(5) . ?
S1 Bi1 2.8108(14) 2_546 ?
S1 C1 1.639(5) . ?
N2 C2 1.154(6) . ?
N3 C3 1.140(6) . ?
N1 C1 1.146(6) . ?

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
S3 Bi1 S3 180.00(6) 1_455 3_676 ?
S3 Bi1 S2 82.18(4) 3_676 . ?
S3 Bi1 S2 82.18(4) 1_455 3_576 ?
S3 Bi1 S2 97.82(4) 3_676 3_576 ?
S3 Bi1 S2 97.82(4) 1_455 . ?
S2 Bi1 S2 180.0 . 3_576 ?
S1 Bi1 S3 85.16(5) 4_575 1_455 ?
S1 Bi1 S3 85.16(5) 2_556 3_676 ?
S1 Bi1 S3 94.84(5) 2_556 1_455 ?
S1 Bi1 S3 94.84(5) 4_575 3_676 ?
S1 Bi1 S2 83.10(5) 4_575 . ?
S1 Bi1 S2 83.10(5) 2_556 3_576 ?
S1 Bi1 S2 96.90(5) 2_556 . ?
S1 Bi1 S2 96.90(5) 4_575 3_576 ?
S1 Bi1 S1 180.0 4_575 2_556 ?
N2 Fe1 N2 180.0 3_666 . ?
N3 Fe1 N2 88.35(16) 3_666 . ?
N3 Fe1 N2 91.66(16) 3_666 3_666 ?
N3 Fe1 N2 91.65(16) . . ?
N3 Fe1 N2 88.34(16) . 3_666 ?
N3 Fe1 N3 180.0 3_666 . ?
N1 Fe1 N2 89.47(17) . . ?
N1 Fe1 N2 89.47(17) 3_666 3_666 ?
N1 Fe1 N2 90.53(17) . 3_666 ?
N1 Fe1 N2 90.54(17) 3_666 . ?
N1 Fe1 N3 90.45(17) 3_666 . ?
N1 Fe1 N3 89.55(17) 3_666 3_666 ?
N1 Fe1 N3 89.55(17) . . ?
N1 Fe1 N3 90.45(17) . 3_666 ?
N1 Fe1 N1 180.0 . 3_666 ?
C3 S3 Bi1 96.22(16) . 1_655 ?
C2 S2 Bi1 98.20(16) . . ?
C1 S1 Bi1 98.64(17) . 2_546 ?
C2 N2 Fe1 169.4(4) . . ?
C3 N3 Fe1 171.2(4) . . ?
C1 N1 Fe1 174.6(4) . . ?
N3 C3 S3 179.3(5) . . ?
N2 C2 S2 178.7(4) . . ?
N1 C1 S1 178.1(4) . . ?

_iucr_refine_instructions_details 
;

    import.res created by SHELXL-2014/7

TITL import_a.res in P2(1)/n
REM Old TITL import in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.102, Rweak 0.001, Alpha 0.029, Orientation as input
REM Formula found by SHELXT: Fe Bi S6 C6 N6
CELL 0.71073 8.384 8.4926 12.1272 90 90.06 90
ZERR 2 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Bi C Fe N S
UNIT 2 12 2 12 12
 
L.S. 10
PLAN  20
TEMP 26.85
BOND $H
list 4
fmap 2
acta
OMIT 0 1 1
OMIT 1 0 1
OMIT -1 0 1
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%./import.hkl">
REM </olex2.extras>
 
WGHT    0.029700    1.737600
FVAR       0.47976
BI1   1    0.000000    1.000000    0.500000    10.50000    0.02473    0.03502 =
         0.02527   -0.00145    0.00057   -0.00088
FE1   3    0.500000    0.500000    0.500000    10.50000    0.02157    0.03347 =
         0.02519   -0.00127   -0.00129    0.00061
S3    5    1.018857    0.699831    0.401476    11.00000    0.02929    0.04483 =
         0.08288   -0.01520    0.01788   -0.00446
S2    5    0.253045    0.964171    0.651625    11.00000    0.06550    0.06566 =
         0.04550   -0.02088   -0.01712    0.03280
S1    5    0.747572    0.418386    0.854722    11.00000    0.04708    0.13622 =
         0.02864    0.00769   -0.00140    0.04481
N2    4    0.408057    0.711836    0.552180    11.00000    0.03508    0.03859 =
         0.04693   -0.00837   -0.00406    0.00512
N3    4    0.710654    0.603956    0.454779    11.00000    0.02751    0.04046 =
         0.04451   -0.00133    0.00207   -0.00421
N1    4    0.590579    0.463119    0.654694    11.00000    0.03554    0.05705 =
         0.03075    0.00086   -0.00115    0.00583
C3    2    0.836621    0.644008    0.433371    11.00000    0.03382    0.03312 =
         0.03511   -0.00338    0.00186    0.00190
C2    2    0.342676    0.816625    0.592432    11.00000    0.03137    0.04103 =
         0.03555   -0.00056   -0.00707    0.00397
C1    2    0.652941    0.445328    0.737921    11.00000    0.03259    0.04953 =
         0.03250   -0.00013    0.00321    0.01143
HKLF 4
 
REM  import_a.res in P2(1)/n
REM R1 =  0.0274 for    1754 Fo > 4sig(Fo)  and  0.0323 for all    1969 data
REM     94 parameters refined using      0 restraints
 
END  
     
WGHT      0.0297      1.7566 

REM Highest difference peak  0.635,  deepest hole -1.410,  1-sigma level  0.194
Q1    1   0.6720  0.3277  0.8378  11.00000  0.05    0.63
Q2    1   0.1961  0.8636  0.6718  11.00000  0.05    0.52
Q3    1   1.0945  0.8824  0.3571  11.00000  0.05    0.48
Q4    1   0.9189  0.8069  0.3172  11.00000  0.05    0.45
Q5    1   0.9421  0.8375  0.3391  11.00000  0.05    0.42
Q6    1   0.6026  0.4346  0.8960  11.00000  0.05    0.40
Q7    1   0.1091  0.7740  0.6637  11.00000  0.05    0.39
Q8    1   0.1015  0.8273  0.6193  11.00000  0.05    0.37
Q9    1   0.3474  0.7325  0.7381  11.00000  0.05    0.35
Q10   1   0.1806  0.9722  0.5057  11.00000  0.05    0.34
Q11   1   0.1829  1.1232  0.5832  11.00000  0.05    0.34
Q12   1   0.9291  0.7135  0.3583  11.00000  0.05    0.33
Q13   1   0.8926  0.8157  0.4005  11.00000  0.05    0.33
Q14   1   0.0516  1.1223  0.5780  11.00000  0.05    0.33
Q15   1   0.6165  0.6537  0.7806  11.00000  0.05    0.32
Q16   1   0.7642  0.5017  0.8211  11.00000  0.05    0.32
Q17   1   0.5542  0.3328  0.8502  11.00000  0.05    0.31
Q18   1   0.1234  0.8662  0.4991  11.00000  0.05    0.31
Q19   1   1.1138  0.7637  0.3316  11.00000  0.05    0.30
Q20   1   0.4093  0.3781  0.7073  11.00000  0.05    0.30

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0274 for 1754 Fo > 4sig(Fo) and 0.0323 for all 3933 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.63, deepest hole -1.41
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0323
  REM R1_gt = 0.0274
  REM wR_ref = 0.0690
  REM GOOF = 1.234
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3933
  REM Reflections_gt = 1754
  REM Parameters = n/a
  REM Hole = -1.41
  REM Peak = 0.63
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'


#==============================================================================
# start Validation Reply Forms
#==============================================================================
_vrf_PLAT241_ALERT_2_C           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S2 Check 
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_ALERT_2_C           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check 
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
#==============================================================================
#==============================================================================
_vrf_PLAT906_ALERT_3_C           
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.830 Check
RESPONSE: The most common place for a high value of K is in the lowest-
intensity bin in the table. Almost all area detector integration programs end 
up slightly underestimating the background, resulting in overestimated values 
of Fo, thus the high value of Fo/Fc. This is most obvious in the weakest 
intensities, since the small addition to Fo becomes insignificant in the ratio 
when Fo is large.
;
#==============================================================================
#==============================================================================
# end Validation Reply Forms
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FeBiSCN6_375K
_database_code_depnum_ccdc_archive 'CCDC 1860299'
_audit_update_record             
;
2018-08-05 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT157_FeBiSCN6_375K       
;
PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg        89.95 Degree
RESPONSE: Chosen to be consistent with other structures.
;
_vrf_PLAT241_FeBiSCN6_375K       
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S2 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_FeBiSCN6_375K       
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Fe1 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_FeBiSCN6_375K_2     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_FeBiSCN6_375K_3     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C2 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
# Added during the CSD deposition process: Sunday 05 August 2018 01:39 PM
# end Validation Reply Form

_audit_creation_date             2018-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'iron(III) hexathiocyanatobismuthate'
_chemical_formula_moiety         '0.5(Bi2 C12 Fe2 N12 S12)'
_chemical_formula_sum            'C6 Bi Fe N6 S6'
_chemical_formula_weight         613.31
_chemical_melting_point          decomposes
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.38360(10)
_cell_length_b                   8.51830(10)
_cell_length_c                   12.1478(2)
_cell_angle_alpha                90
_cell_angle_beta                 89.9500(10)
_cell_angle_gamma                90
_cell_volume                     867.52(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2094
_cell_measurement_temperature    375(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_diffrn_measurement_method       CCD

_exptl_absorpt_coefficient_mu    11.681
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             566

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16

_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3763
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         3.354
_diffrn_ambient_temperature      375(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'

_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1634
_reflns_number_total             1973
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.921
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1973
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+1.4377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0766

_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 1.0000 0.0000 0.5000 0.03501(11) Uani 1 2 d S T P . .
Fe1 Fe 0.5000 0.5000 0.5000 0.0332(2) Uani 1 2 d S T P . .
S3 S -0.01760(16) 0.29893(19) 0.59901(15) 0.0638(4) Uani 1 1 d . . . . .
S2 S 0.7457(3) 0.0362(2) 0.34976(16) 0.0719(5) Uani 1 1 d . . . . .
S1 S 0.2535(2) 0.5812(3) 0.14623(13) 0.0864(7) Uani 1 1 d . . . . .
N3 N 0.2889(5) 0.3965(5) 0.5452(4) 0.0461(10) Uani 1 1 d . . . . .
N2 N 0.5922(5) 0.2884(6) 0.4480(4) 0.0505(11) Uani 1 1 d . . . . .
N1 N 0.4094(6) 0.5373(6) 0.3453(4) 0.0498(11) Uani 1 1 d . . . . .
C3 C 0.1640(5) 0.3551(6) 0.5667(4) 0.0402(10) Uani 1 1 d . . . . .
C2 C 0.6572(6) 0.1846(6) 0.4088(4) 0.0441(11) Uani 1 1 d . . . . .
C1 C 0.3483(6) 0.5537(8) 0.2629(4) 0.0462(12) Uani 1 1 d . . . . .

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
Bi1 0.03148(15) 0.04271(17) 0.03083(15) -0.00151(10) 0.00061(9) -0.00132(9)
Fe1 0.0273(4) 0.0411(5) 0.0312(5) -0.0019(4) -0.0018(4) 0.0005(3)
S3 0.0370(6) 0.0554(8) 0.0991(12) -0.0193(8) 0.0216(7) -0.0054(6)
S2 0.0803(12) 0.0809(11) 0.0547(10) -0.0258(9) -0.0227(8) 0.0402(10)
S1 0.0582(9) 0.165(2) 0.0362(7) 0.0092(11) -0.0012(6) 0.0537(12)
N3 0.036(2) 0.049(3) 0.054(3) -0.003(2) 0.0039(18) -0.0081(19)
N2 0.043(2) 0.051(3) 0.057(3) -0.011(2) -0.0042(19) 0.005(2)
N1 0.044(2) 0.071(3) 0.034(2) 0.003(2) -0.0022(19) 0.007(2)
C3 0.039(2) 0.039(3) 0.042(3) -0.002(2) 0.0013(19) 0.001(2)
C2 0.040(2) 0.051(3) 0.041(3) -0.002(2) -0.010(2) 0.005(2)
C1 0.043(3) 0.062(3) 0.034(3) 0.002(2) 0.003(2) 0.018(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Bi1 S3 2.8199(15) 1_655 ?
Bi1 S3 2.8199(15) 3_656 ?
Bi1 S2 2.8244(17) 3_756 ?
Bi1 S2 2.8244(17) . ?
Bi1 S1 2.8107(16) 4_666 ?
Bi1 S1 2.8107(16) 2_645 ?
Fe1 N3 2.051(4) 3_666 ?
Fe1 N3 2.052(4) . ?
Fe1 N2 2.060(5) . ?
Fe1 N2 2.060(5) 3_666 ?
Fe1 N1 2.053(5) 3_666 ?
Fe1 N1 2.053(5) . ?
S3 Bi1 2.8200(15) 1_455 ?
S3 C3 1.643(5) . ?
S2 C2 1.632(6) . ?
S1 Bi1 2.8106(16) 2_655 ?
S1 C1 1.643(5) . ?
N3 C3 1.135(6) . ?
N2 C2 1.142(6) . ?
N1 C1 1.133(7) . ?

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
S3 Bi1 S3 180.0 1_655 3_656 ?
S3 Bi1 S2 97.93(5) 3_656 3_756 ?
S3 Bi1 S2 97.93(5) 1_655 . ?
S3 Bi1 S2 82.07(5) 3_656 . ?
S3 Bi1 S2 82.07(5) 1_655 3_756 ?
S2 Bi1 S2 180.00(8) 3_756 . ?
S1 Bi1 S3 85.09(6) 4_666 1_655 ?
S1 Bi1 S3 85.09(6) 2_645 3_656 ?
S1 Bi1 S3 94.91(6) 2_645 1_655 ?
S1 Bi1 S3 94.91(6) 4_666 3_656 ?
S1 Bi1 S2 96.88(6) 4_666 3_756 ?
S1 Bi1 S2 83.12(6) 4_666 . ?
S1 Bi1 S2 83.12(6) 2_645 3_756 ?
S1 Bi1 S2 96.88(6) 2_645 . ?
S1 Bi1 S1 180.0 4_666 2_645 ?
N3 Fe1 N3 180.0 3_666 . ?
N3 Fe1 N2 91.69(18) 3_666 3_666 ?
N3 Fe1 N2 91.69(18) . . ?
N3 Fe1 N2 88.31(18) . 3_666 ?
N3 Fe1 N2 88.32(18) 3_666 . ?
N3 Fe1 N1 89.54(19) 3_666 3_666 ?
N3 Fe1 N1 90.46(19) . 3_666 ?
N3 Fe1 N1 90.46(19) 3_666 . ?
N3 Fe1 N1 89.54(19) . . ?
N2 Fe1 N2 180.0(2) 3_666 . ?
N1 Fe1 N2 89.7(2) 3_666 3_666 ?
N1 Fe1 N2 90.3(2) . 3_666 ?
N1 Fe1 N2 90.3(2) 3_666 . ?
N1 Fe1 N2 89.7(2) . . ?
N1 Fe1 N1 180.0 3_666 . ?
C3 S3 Bi1 96.48(18) . 1_455 ?
C2 S2 Bi1 98.25(18) . . ?
C1 S1 Bi1 98.86(18) . 2_655 ?
C3 N3 Fe1 172.0(4) . . ?
C2 N2 Fe1 169.6(5) . . ?
C1 N1 Fe1 174.6(5) . . ?
N3 C3 S3 178.7(5) . . ?
N2 C2 S2 178.2(5) . . ?
N1 C1 S1 177.5(5) . . ?

_iucr_refine_instructions_details 
;

    import.res created by SHELXL-2014/7

TITL import_a.res in P2(1)/n
REM Old TITL GLOBAL OLEX2: imported from CIF
REM SHELXT solution in P2(1)/n
REM R1 0.114, Rweak 0.002, Alpha 0.028, Orientation as input
REM Formula found by SHELXT: Fe Bi S6 C6 N6
CELL 0.71073 8.3836 8.5183 12.1478 90 89.95 90
ZERR 2 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Bi C Fe N S
UNIT 2 12 2 12 12
 
L.S. 10
PLAN  20
TEMP 101.85
BOND $H
list 4
fmap 2
acta
OMIT -1 0 1
OMIT 1 0 1
OMIT -1 0 1
OMIT 0 1 1
OMIT 1 1 0
OMIT -2 3 3
REM <olex2.extras>
REM <HklSrc "%./beta_prime.hkl">
REM </olex2.extras>
 
WGHT    0.035300    1.437700
FVAR       0.37882
BI1   1    1.000000    0.000000    0.500000    10.50000    0.03148    0.04271 =
         0.03083   -0.00151    0.00061   -0.00132
FE1   3    0.500000    0.500000    0.500000    10.50000    0.02727    0.04111 =
         0.03124   -0.00194   -0.00183    0.00052
S3    5   -0.017596    0.298931    0.599014    11.00000    0.03697    0.05538 =
         0.09910   -0.01929    0.02157   -0.00543
S2    5    0.745723    0.036166    0.349759    11.00000    0.08025    0.08088 =
         0.05474   -0.02583   -0.02270    0.04024
S1    5    0.253452    0.581191    0.146230    11.00000    0.05817    0.16490 =
         0.03615    0.00922   -0.00117    0.05368
N3    4    0.288929    0.396504    0.545234    11.00000    0.03553    0.04939 =
         0.05352   -0.00318    0.00394   -0.00814
N2    4    0.592203    0.288379    0.448005    11.00000    0.04342    0.05111 =
         0.05685   -0.01086   -0.00423    0.00526
N1    4    0.409382    0.537343    0.345280    11.00000    0.04408    0.07129 =
         0.03405    0.00260   -0.00219    0.00669
C3    2    0.164002    0.355112    0.566661    11.00000    0.03918    0.03888 =
         0.04240   -0.00244    0.00131    0.00065
C2    2    0.657184    0.184600    0.408840    11.00000    0.03996    0.05140 =
         0.04085   -0.00242   -0.01002    0.00509
C1    2    0.348318    0.553699    0.262915    11.00000    0.04264    0.06210 =
         0.03397    0.00199    0.00343    0.01756
HKLF 4
 
REM  import_a.res in P2(1)/n
REM R1 =  0.0296 for    1634 Fo > 4sig(Fo)  and  0.0379 for all    1973 data
REM     94 parameters refined using      0 restraints
 
END  
     
WGHT      0.0355      1.4192 

REM Highest difference peak  0.921,  deepest hole -1.533,  1-sigma level  0.210
Q1    1   0.3311  0.6818  0.1622  11.00000  0.05    0.92
Q2    1   0.8017  0.1417  0.3253  11.00000  0.05    0.53
Q3    1   0.1083  0.1772  0.6949  11.00000  0.05    0.45
Q4    1   0.6525  0.3234  0.2785  11.00000  0.05    0.43
Q5    1   0.8801  0.1785  0.3999  11.00000  0.05    0.43
Q6    1   0.3954  0.2549  0.6833  11.00000  0.05    0.41
Q7    1   0.1245  0.1860  0.6052  11.00000  0.05    0.41
Q8    1   0.3844  0.4740  0.1504  11.00000  0.05    0.40
Q9    1   0.8795  0.2103  0.3292  11.00000  0.05    0.39
Q10   1   0.6363  0.2590  0.2434  11.00000  0.05    0.38
Q11   1  -0.0683  0.1115  0.6513  11.00000  0.05    0.38
Q12   1  -0.1089  0.2218  0.7535  11.00000  0.05    0.37
Q13   1   0.5952  0.6214  0.2946  11.00000  0.05    0.37
Q14   1   0.6176  0.4225  0.3221  11.00000  0.05    0.37
Q15   1   1.1202 -0.1206  0.5271  11.00000  0.05    0.37
Q16   1   0.8783  0.1163  0.3621  11.00000  0.05    0.36
Q17   1   0.3869  0.3370  0.2178  11.00000  0.05    0.34
Q18   1  -0.0959  0.2442  0.6745  11.00000  0.05    0.34
Q19   1   0.8762 -0.1000  0.3612  11.00000  0.05    0.34
Q20   1   0.2422  0.4970  0.1768  11.00000  0.05    0.34

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0296 for 1634 Fo > 4sig(Fo) and 0.0379 for all 3916 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.92, deepest hole -1.53
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0379
  REM R1_gt = 0.0296
  REM wR_ref = 0.0766
  REM GOOF = 1.188
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3916
  REM Reflections_gt = 1634
  REM Parameters = n/a
  REM Hole = -1.53
  REM Peak = 0.92
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'



#==============================================================================
# start Validation Reply Forms
#==============================================================================

_vrf_PLAT157_ALERT_4_C           
;
PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg        89.95 Degree
RESPONSE: Chosen to be consistent with other structures.
;
#==============================================================================
#==============================================================================
_vrf_PLAT241_ALERT_2_C           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S2 Check 
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
_vrf_PLAT242_ALERT_2_C           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Fe1 Check 
         Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check 
         Low    'MainMol' Ueq as Compared to Neighbors of         C2 Check 
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
#==============================================================================
#==============================================================================
_vrf_PLAT906_ALERT_3_C           
;
PROBLEM: Large K Value in the Analysis of Variance ......      6.550 Check
RESPONSE: The most common place for a high value of K is in the lowest-
intensity bin in the table. Almost all area detector integration programs end 
up slightly underestimating the background, resulting in overestimated values 
of Fo, thus the high value of Fo/Fc. This is most obvious in the weakest 
intensities, since the small addition to Fo becomes insignificant in the ratio 
when Fo is large.
;
#==============================================================================
#==============================================================================
_vrf_PLAT974_ALERT_2_C           
;
PROBLEM: Check Calcd Negative Resid. Density on       Bi1      -1.16 eA-3 
RESPONSE: It is common for residual density to remain near heavy atoms, due to 
fourier termination ripples.
;
#==============================================================================
#==============================================================================
# end Validation Reply Forms
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ScBiSCN6
_database_code_depnum_ccdc_archive 'CCDC 1860298'
_audit_update_record             
;
2018-08-05 deposited with the CCDC.
2018-10-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT241_ScBiSCN6            
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       S004 Check
RESPONSE: The sulfur atoms show considerably more motion than the adjacent  heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
# Added during the CSD deposition process: Sunday 05 August 2018 01:39 PM
# end Validation Reply Form

_audit_creation_date             2018-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            'scandium(III) hexathiocyanatobismuthate'
_chemical_formula_moiety         '0.5(C12 Bi2 N12 S12 Sc2)'
_chemical_formula_sum            'C6 Bi1 N6 S6 Sc1'
_chemical_formula_weight         602.42
_chemical_melting_point          decomposes
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.4782(2)
_cell_length_b                   8.6324(2)
_cell_length_c                   12.2676(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.3450(10)
_cell_angle_gamma                90
_cell_volume                     897.82(4)
_cell_formula_units_Z            2

_cell_measurement_reflns_used    2135
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485
_cell_measurement_temperature    180(2)
_diffrn_measurement_method       CCD
_exptl_absorpt_coefficient_mu    10.857
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.228
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3766
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.912
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       KappaCCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1621
_reflns_number_total             2032
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.424
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2032
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0286
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+0.8072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0669



_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi01 Bi 0.0000 1.0000 0.5000 0.02499(10) Uani 1 2 d S T P . .
Sc02 Sc 0.5000 0.5000 0.5000 0.0226(2) Uani 1 2 d S T P . .
S003 S 1.02578(14) 0.70558(15) 0.40180(12) 0.0417(3) Uani 1 1 d . . . . .
S004 S 0.24556(18) 0.96665(17) 0.65464(11) 0.0448(4) Uani 1 1 d . . . . .
S005 S 0.74961(16) 0.4171(2) 0.86191(10) 0.0526(4) Uani 1 1 d . . . . .
N006 N 0.7212(4) 0.6073(4) 0.4523(3) 0.0304(8) Uani 1 1 d . . . . .
N007 N 0.5981(5) 0.4612(5) 0.6617(3) 0.0349(10) Uani 1 1 d . . . . .
N008 N 0.4038(4) 0.7191(5) 0.5563(3) 0.0352(9) Uani 1 1 d . . . . .
C009 C 0.8458(5) 0.6488(5) 0.4322(3) 0.0297(10) Uani 1 1 d . . . . .
C00A C 0.3365(5) 0.8214(6) 0.5956(4) 0.0303(10) Uani 1 1 d . . . . .
C00B C 0.6586(5) 0.4450(6) 0.7448(4) 0.0322(10) Uani 1 1 d . . . . .

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
Bi01 0.02168(14) 0.03193(15) 0.02137(13) -0.00247(10) -0.00024(8) -0.00100(9)
Sc02 0.0189(5) 0.0298(6) 0.0190(5) -0.0017(5) -0.0021(4) 0.0001(4)
S003 0.0257(6) 0.0380(7) 0.0614(9) -0.0122(6) 0.0118(5) -0.0023(5)
S004 0.0491(8) 0.0548(9) 0.0305(7) -0.0131(6) -0.0102(6) 0.0227(6)
S005 0.0374(7) 0.0971(12) 0.0233(6) 0.0063(7) -0.0018(5) 0.0298(8)
N006 0.025(2) 0.034(2) 0.032(2) -0.0028(17) 0.0010(15) -0.0033(17)
N007 0.032(2) 0.050(3) 0.023(2) 0.0033(18) -0.0015(17) 0.0069(18)
N008 0.030(2) 0.041(2) 0.035(2) -0.0033(19) -0.0064(17) 0.0030(18)
C009 0.029(2) 0.032(3) 0.028(2) -0.0048(19) 0.0000(18) 0.006(2)
C00A 0.026(2) 0.036(3) 0.028(2) 0.002(2) -0.0077(18) 0.002(2)
C00B 0.028(2) 0.037(2) 0.032(3) 0.004(2) 0.0043(19) 0.012(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Bi01 S003 2.8217(13) 1_455 ?
Bi01 S003 2.8217(13) 3_676 ?
Bi01 S004 2.8228(14) . ?
Bi01 S004 2.8229(14) 3_576 ?
Bi01 S005 2.8113(13) 4_575 ?
Bi01 S005 2.8113(13) 2_556 ?
Sc02 N006 2.175(4) . ?
Sc02 N006 2.175(4) 3_666 ?
Sc02 N007 2.172(4) 3_666 ?
Sc02 N007 2.172(4) . ?
Sc02 N008 2.174(4) 3_666 ?
Sc02 N008 2.175(4) . ?
S003 Bi01 2.8217(13) 1_655 ?
S003 C009 1.648(5) . ?
S004 C00A 1.643(5) . ?
S005 Bi01 2.8113(13) 2_546 ?
S005 C00B 1.645(5) . ?
N006 C009 1.144(5) . ?
N007 C00B 1.147(6) . ?
N008 C00A 1.157(6) . ?

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
S003 Bi01 S003 180.00(5) 1_455 3_676 ?
S003 Bi01 S004 82.17(4) 3_676 . ?
S003 Bi01 S004 82.17(4) 1_455 3_576 ?
S003 Bi01 S004 97.83(4) 3_676 3_576 ?
S003 Bi01 S004 97.83(4) 1_455 . ?
S004 Bi01 S004 180.0 . 3_576 ?
S005 Bi01 S003 84.92(5) 4_575 1_455 ?
S005 Bi01 S003 84.92(5) 2_556 3_676 ?
S005 Bi01 S003 95.08(5) 2_556 1_455 ?
S005 Bi01 S003 95.08(5) 4_575 3_676 ?
S005 Bi01 S004 82.88(4) 4_575 . ?
S005 Bi01 S004 97.12(4) 4_575 3_576 ?
S005 Bi01 S004 97.12(4) 2_556 . ?
S005 Bi01 S004 82.88(4) 2_556 3_576 ?
S005 Bi01 S005 180.0 4_575 2_556 ?
N006 Sc02 N006 180.0 . 3_666 ?
N007 Sc02 N006 90.83(15) . 3_666 ?
N007 Sc02 N006 89.17(15) . . ?
N007 Sc02 N006 90.83(15) 3_666 . ?
N007 Sc02 N006 89.17(15) 3_666 3_666 ?
N007 Sc02 N007 180.0(2) 3_666 . ?
N007 Sc02 N008 90.78(15) . 3_666 ?
N007 Sc02 N008 89.22(15) 3_666 3_666 ?
N007 Sc02 N008 90.78(15) 3_666 . ?
N007 Sc02 N008 89.22(15) . . ?
N008 Sc02 N006 92.33(14) 3_666 3_666 ?
N008 Sc02 N006 87.67(14) 3_666 . ?
N008 Sc02 N006 92.33(14) . . ?
N008 Sc02 N006 87.67(14) . 3_666 ?
N008 Sc02 N008 180.00(11) 3_666 . ?
C009 S003 Bi01 95.57(16) . 1_655 ?
C00A S004 Bi01 97.34(15) . . ?
C00B S005 Bi01 97.95(17) . 2_546 ?
C009 N006 Sc02 172.0(4) . . ?
C00B N007 Sc02 175.6(4) . . ?
C00A N008 Sc02 169.2(4) . . ?
N006 C009 S003 178.9(4) . . ?
N008 C00A S004 178.1(4) . . ?
N007 C00B S005 177.9(5) . . ?

_iucr_refine_instructions_details 
;

    import.res created by SHELXL-2014/7

TITL import_a.res in P2(1)/n
REM Old TITL import in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.099, Rweak 0.002, Alpha 0.021, Orientation as input
REM Formula found by SHELXT: Sc Bi S6 C6 N6
CELL 0.71073 8.4782 8.6324 12.2676 90 90.345 90
ZERR 2 0.0002 0.0002 0.0003 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC Bi C N S Sc
UNIT 2 12 12 12 2
 
L.S. 4
PLAN  20
BOND $H
list 4
fmap 2
ACTA
OMIT 1 1 0
OMIT 0 0 2
OMIT 0 1 1
OMIT 1 0 1
OMIT 1 1 1
OMIT -1 1 1
REM <olex2.extras>
REM <HklSrc "%./import.hkl">
REM </olex2.extras>
 
WGHT    0.030700    0.807200
FVAR       0.45735
BI01  1    0.000000    1.000000    0.500000    10.50000    0.02168    0.03193 =
         0.02137   -0.00247   -0.00024   -0.00100
SC02  5    0.500000    0.500000    0.500000    10.50000    0.01886    0.02978 =
         0.01899   -0.00171   -0.00209    0.00008
S003  4    1.025779    0.705576    0.401801    11.00000    0.02573    0.03805 =
         0.06144   -0.01216    0.01177   -0.00235
S004  4    0.245563    0.966645    0.654636    11.00000    0.04914    0.05476 =
         0.03047   -0.01308   -0.01022    0.02269
S005  4    0.749614    0.417123    0.861912    11.00000    0.03740    0.09708 =
         0.02334    0.00630   -0.00176    0.02975
N006  3    0.721159    0.607315    0.452278    11.00000    0.02536    0.03406 =
         0.03186   -0.00282    0.00095   -0.00326
N007  3    0.598099    0.461179    0.661654    11.00000    0.03161    0.04982 =
         0.02326    0.00330   -0.00148    0.00692
N008  3    0.403782    0.719148    0.556322    11.00000    0.03016    0.04060 =
         0.03490   -0.00327   -0.00636    0.00299
C009  2    0.845775    0.648807    0.432206    11.00000    0.02886    0.03244 =
         0.02795   -0.00483    0.00002    0.00566
C00A  2    0.336530    0.821414    0.595578    11.00000    0.02612    0.03646 =
         0.02835    0.00223   -0.00769    0.00177
C00B  2    0.658604    0.445003    0.744760    11.00000    0.02764    0.03735 =
         0.03153    0.00378    0.00426    0.01156
HKLF 4
 
REM  import_a.res in P2(1)/n
REM R1 =  0.0286 for    1621 Fo > 4sig(Fo)  and  0.0406 for all    2032 data
REM     94 parameters refined using      0 restraints
 
END  
     
WGHT      0.0305      0.8193 

REM Highest difference peak  1.424,  deepest hole -1.111,  1-sigma level  0.152
Q1    1   0.1096  1.0025  0.4803  11.00000  0.05    1.42
Q2    1   0.6820  0.2222  0.7746  11.00000  0.05    0.47
Q3    1   0.3238  0.7198  0.6050  11.00000  0.05    0.46
Q4    1   0.7572  0.5739  0.8627  11.00000  0.05    0.45
Q5    1   0.2415  0.9938  0.5171  11.00000  0.05    0.43
Q6    1   0.6505  0.2632  0.8582  11.00000  0.05    0.42
Q7    1   1.0858  0.7990  0.4067  11.00000  0.05    0.41
Q8    1   0.6759  0.4782  0.8888  11.00000  0.05    0.41
Q9    1   0.9264  0.6034  0.3976  11.00000  0.05    0.41
Q10   1   1.1192  0.7937  0.4948  11.00000  0.05    0.41
Q11   1   0.6764  0.7362  0.5544  11.00000  0.05    0.41
Q12   1   1.1692  0.7043  0.4932  11.00000  0.05    0.40
Q13   1   0.3705  0.6698  0.5184  11.00000  0.05    0.40
Q14   1   0.4896  0.2261  0.8363  11.00000  0.05    0.40
Q15   1   0.7447  0.6779  0.4446  11.00000  0.05    0.39
Q16   1   0.4056  0.4167  0.5150  11.00000  0.05    0.38
Q17   1   0.8523  0.5061  0.7546  11.00000  0.05    0.37
Q18   1   0.8324  0.3754  0.7261  11.00000  0.05    0.37
Q19   1   0.8720  0.6039  0.7379  11.00000  0.05    0.37
Q20   1   0.6034  0.1690  0.8407  11.00000  0.05    0.37

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0286 for 1621 Fo > 4sig(Fo) and 0.0406 for all 3911 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.42, deepest hole -1.11
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0406
  REM R1_gt = 0.0286
  REM wR_ref = 0.0669
  REM GOOF = 1.093
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3911
  REM Reflections_gt = 1621
  REM Parameters = n/a
  REM Hole = -1.11
  REM Peak = 1.42
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'


#==============================================================================
# start Validation Reply Forms
#==============================================================================
_vrf_PLAT241_ALERT_2_C           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       S004 Check 
RESPONSE: The sulfur atoms show considerably more motion than the adjacent 
heavy metal sites and rigid CN groups. This is common for thiocyanate ligands.
;
#==============================================================================
#==============================================================================
_vrf_PLAT906_ALERT_3_C           
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.946 Check 
RESPONSE: The most common place for a high value of K is in the lowest-
intensity bin in the table. Almost all area detector integration programs end 
up slightly underestimating the background, resulting in overestimated values 
of Fo, thus the high value of Fo/Fc. This is most obvious in the weakest 
intensities, since the small addition to Fo becomes insignificant in the ratio 
when Fo is large.
;
#==============================================================================
#==============================================================================
_vrf_PLAT911_ALERT_3_C           
;
PROLBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
RESPONSE: Low angle reflections obscured by beam stop
;
#==============================================================================
#==============================================================================

# end Validation Reply Forms
