#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:16:29 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263673 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/01/1560105.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1560105
loop_
_publ_author_name
'Lee, Jie Yie'
'Ling, Sanliang'
'Argent, Stephen P.'
'Senn, Mark S.'
'Cañadillas-Delgado, Laura'
'Cliffe, Matthew J.'
_publ_section_title
;
 Controlling multiple orderings in metal thiocyanate molecular perovskites
 Ax{Ni[Bi(SCN)6]}
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3516
_journal_page_last               3525
_journal_paper_doi               10.1039/D0SC06619B
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C N S, C H6 N3'
_chemical_formula_sum            'C2 H6 N4 S'
_chemical_formula_weight         118.17
_chemical_name_systematic        'guanidinium thiocyanate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.894(5)
_cell_angle_beta                 104.311(7)
_cell_angle_gamma                101.787(7)
_cell_formula_units_Z            4
_cell_length_a                   6.9352(6)
_cell_length_b                   7.0096(5)
_cell_length_c                   12.3675(7)
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.4830
_cell_measurement_theta_min      3.6280
_cell_volume                     568.89(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1806
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  32.00   1.00    1.00    --  -41.93  38.00 150.00   82
  2  ω    -92.00  -2.00   1.00    1.00    --  -41.93 125.00-150.00   90
  3  ω   -115.00 -14.00   1.00    1.00    --  -41.93 -57.00   0.00  101
  4  ω    -38.00  83.00   1.00    1.00    --   41.93 -19.00 -60.00  121
  5  ω      1.00  83.00   1.00    1.00    --   41.93 -99.00-120.00   82
  6  ω     80.00 178.00   1.00    1.86    --  105.94  45.00 -90.00   98
  7  ω     33.00  98.00   1.00    1.86    --  105.94 -45.00  60.00   65
  8  ω     27.00 111.00   1.00    1.86    --  105.94-103.00  68.00   84
  9  ω     30.00  91.00   1.00    1.86    --  105.94 -30.00   0.00   61
 10  ω     30.00  91.00   1.00    1.86    --  105.94 -30.00 150.00   61
 11  ω     24.00 110.00   1.00    1.86    --  105.94 -95.00 -60.00   86
 12  ω     33.00  98.00   1.00    1.86    --  105.94 -45.00 -60.00   65
 13  ω     33.00 118.00   1.00    1.86    --  105.94-125.00-150.00   85
 14  ω     30.00 139.00   1.00    1.86    --  105.94 -77.00-150.00  109
 15  ω     18.00 178.00   1.00    1.86    --  105.94   0.00-120.00  160
 16  ω     30.00  91.00   1.00    1.86    --  105.94 -30.00-120.00   61
 17  ω     94.00 178.00   1.00    1.86    --  105.94 125.00-120.00   84
 18  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00  30.00  109
 19  ω   -115.00 -14.00   1.00    1.00    --  -41.93 -57.00 150.00  101
 20  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00 120.00  109
 21  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00 -30.00  109
 22  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00-120.00  109
 23  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 -60.00  101
 24  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 -30.00  101
 25  ω     53.00 178.00   1.00    1.86    --  105.94  15.00  60.00  125
 26  ω     73.00 178.00   1.00    1.86    --  105.94  77.00  30.00  105
 27  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 150.00  101
 28  ω     73.00 178.00   1.00    1.86    --  105.94  77.00-180.00  105
 29  ω     73.00 178.00   1.00    1.86    --  105.94  77.00-150.00  105
 30  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 120.00  101
 31  ω     73.00 178.00   1.00    1.86    --  105.94  77.00   0.00  105
 32  ω     77.00 178.00   1.00    1.86    --  105.94  61.00  90.00  101
 33  ω   -116.00 -42.00   1.00    1.00    --  -41.93 -38.00-150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2179114000
_diffrn_orient_matrix_UB_12      -0.0153606000
_diffrn_orient_matrix_UB_13      0.0613508000
_diffrn_orient_matrix_UB_21      0.0703046000
_diffrn_orient_matrix_UB_22      0.0477463000
_diffrn_orient_matrix_UB_23      -0.1071752000
_diffrn_orient_matrix_UB_31      0.0516811000
_diffrn_orient_matrix_UB_32      0.2193997000
_diffrn_orient_matrix_UB_33      0.0368301000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2392
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.681
_diffrn_reflns_theta_min         3.697
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.110
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       irregular
_exptl_crystal_F_000             248
_exptl_crystal_preparation       'as received'
_exptl_crystal_recrystallization_method 'from bottle'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0898
_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)+(0.1190P)²+3.4535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1975
_reflns_number_total             2256
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc06619b3.cif
_cod_data_source_block           GuaSCN
_cod_depositor_comments
'Adding full bibliography for 1560103--1560109.cif.'
_cod_original_cell_volume        568.89(7)
_cod_database_code               1560105
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C2 N4 H6 S'
_chemical_oxdiff_usercomment
'omjclb #18016 in fomblin on micromount for MJC'
_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.
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2.a X=CH2 refined with riding coordinates:
 N003(H00A,H00B), N004(H00G,H00H), N005(H00I,H00J), N006(H00C,H00D), N009(H00E,
 H00F), N00A(H00K,H00L)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.211
_oxdiff_exptl_absorpt_empirical_full_min 0.693
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S001 S 0.8059(2) 0.5908(2) 0.68433(11) 0.0325(4) Uani 1 1 d . . . . .
S002 S 0.7722(2) 1.0625(2) 0.91180(11) 0.0290(4) Uani 1 1 d . . . . .
N003 N 0.2574(8) 1.0879(7) 0.5218(4) 0.0307(11) Uani 1 1 d . . . . .
H00A H 0.290753 1.097377 0.593776 0.037 Uiso 1 1 calc R . . . .
H00B H 0.252204 1.191132 0.485500 0.037 Uiso 1 1 calc R . . . .
N004 N 0.2162(7) 0.4249(7) 1.0413(4) 0.0288(10) Uani 1 1 d . . . . .
H00G H 0.201126 0.314716 1.071164 0.035 Uiso 1 1 calc R . . . .
H00H H 0.207173 0.528371 1.076345 0.035 Uiso 1 1 calc R . . . .
N005 N 0.2675(7) 0.2794(7) 0.8862(4) 0.0294(10) Uani 1 1 d . . . . .
H00I H 0.290573 0.287315 0.821031 0.035 Uiso 1 1 calc R . . . .
H00J H 0.253630 0.168714 0.915686 0.035 Uiso 1 1 calc R . . . .
N006 N 0.2222(8) 0.7557(7) 0.5227(4) 0.0329(11) Uani 1 1 d . . . . .
H00C H 0.255469 0.764568 0.594681 0.039 Uiso 1 1 calc R . . . .
H00D H 0.194058 0.643221 0.486863 0.039 Uiso 1 1 calc R . . . .
N007 N 0.3875(8) 0.9529(7) 0.7579(4) 0.0319(11) Uani 1 1 d . . . . .
N008 N 0.3954(8) 0.4573(8) 0.6863(4) 0.0352(12) Uani 1 1 d . . . . .
N009 N 0.1582(8) 0.8994(7) 0.3560(4) 0.0315(11) Uani 1 1 d . . . . .
H00E H 0.149882 1.002086 0.319476 0.038 Uiso 1 1 calc R . . . .
H00F H 0.130219 0.786545 0.320550 0.038 Uiso 1 1 calc R . . . .
N00A N 0.2747(8) 0.6071(7) 0.8954(4) 0.0317(11) Uani 1 1 d . . . . .
H00K H 0.297786 0.615818 0.830271 0.038 Uiso 1 1 calc R . . . .
H00L H 0.265317 0.709307 0.931414 0.038 Uiso 1 1 calc R . . . .
C00B C 0.2535(7) 0.4355(8) 0.9404(4) 0.0237(11) Uani 1 1 d . . . . .
C00C C 0.5448(9) 0.9988(8) 0.8215(4) 0.0274(12) Uani 1 1 d . . . . .
C00D C 0.5628(9) 0.5121(8) 0.6842(4) 0.0286(12) Uani 1 1 d . . . . .
C00E C 0.2144(8) 0.9151(8) 0.4672(4) 0.0255(11) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 5 0.0503
3 -2 5 0.0590
0 4 2 0.0901
-4 0 1 0.0286
-2 -2 7 0.0604
-2 0 8 0.0525
0 4 0 0.0887
2 0 -8 0.0534
1 -4 -3 0.0907
-4 0 -1 0.0248
4 0 0 0.0199
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
N005 C00B N004 120.6(5) . . ?
N005 C00B N00A 120.4(5) . . ?
N00A C00B N004 119.0(5) . . ?
N007 C00C S002 179.2(5) . . ?
N008 C00D S001 178.6(5) . . ?
N003 C00E N006 120.3(5) . . ?
N003 C00E N009 120.2(5) . . ?
N006 C00E N009 119.6(5) . . ?
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
S001 C00D 1.663(6) . ?
S002 C00C 1.661(6) . ?
N003 C00E 1.319(7) . ?
N004 C00B 1.335(7) . ?
N005 C00B 1.308(7) . ?
N006 C00E 1.324(7) . ?
N007 C00C 1.156(8) . ?
N008 C00D 1.153(8) . ?
N009 C00E 1.330(7) . ?
N00A C00B 1.329(7) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.0147 -0.0099 4.9754 0.7444 -0.3921 0.2852
3.0067 -2.0122 4.9779 0.9915 -0.4182 -0.1028
0.0235 3.9971 1.9754 0.0649 -0.0192 0.9509
-4.0032 0.0109 1.0304 -0.8093 -0.3914 -0.1666
-1.9955 -1.9992 7.0146 0.0262 -0.9875 -0.2834
-1.9838 -0.0006 8.0023 0.0587 -0.9971 0.1921
0.0187 3.9988 -0.0212 -0.0586 0.1945 0.8775
1.9838 0.0006 -8.0023 -0.0587 0.9971 -0.1921
0.9756 -3.9993 -2.9817 0.0911 0.1972 -0.9368
-4.0080 0.0125 -0.9662 -0.9329 -0.1776 -0.2400
4.0056 -0.0117 -0.0321 0.8711 0.2845 0.2033
