The structures of ordered defects in thiocyanate analogues of Prussian Blue
Cliffe, Matthew J.; Keyzer, Evan N.; Bond, Andrew D.; Astle, Maxwell A.; Grey, Clare P.; Chemical Science 11 (2020) 4430–4438; doi:10.1039/D0SC01246G

data_1557769
_publ_section_title
;
 The structures of ordered defects in thiocyanate analogues of Prussian
 Blue
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              4430
_journal_page_last               4438
_journal_paper_doi               10.1039/D0SC01246G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C30 H74 Bi5 N33 Ni6 O16 S30'
_chemical_formula_sum            'C30 H74 Bi5 N33 Ni6 O16 S30'
_chemical_formula_weight         3512.13
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-27 deposited with the CCDC.	2020-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                84.0731(7)
_cell_angle_beta                 76.7140(7)
_cell_angle_gamma                85.1942(8)
_cell_formula_units_Z            1
_cell_length_a                   11.8567(2)
_cell_length_b                   11.8653(2)
_cell_length_c                   18.3824(4)
_cell_measurement_reflns_used    10868
_cell_measurement_temperature    111
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2498.60(8)
_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)'
_diffrn_ambient_temperature      111
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius Kappa'
_diffrn_measurement_method       \w/2\q
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.05014
_diffrn_orient_matrix_UB_12      -0.02513
_diffrn_orient_matrix_UB_13      -0.06629
_diffrn_orient_matrix_UB_21      -0.06661
_diffrn_orient_matrix_UB_22      -0.04567
_diffrn_orient_matrix_UB_23      -0.02617
_diffrn_orient_matrix_UB_31      -0.02052
_diffrn_orient_matrix_UB_32      0.04912
_diffrn_orient_matrix_UB_33      -0.01774
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20614
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         2.983
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    10.562
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1610
_exptl_crystal_preparation       'precipitated from acidic solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         11356
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+14.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8490
_reflns_number_total             11356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01246g3.cif
_cod_data_source_block           4_Ni6Bi5NCS30_3NH4
_cod_depositor_comments
;Adding full bibliography for 1557765--1557770.cif.

 Adding full bibliography for 1557765--1557770.cif.
;
_cod_database_code               1557769
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.418
_olex2_refinement_description
;
1. Restrained distances
 N17-H17C
 0.88 with sigma of 0.02
 N17-H17A
 0.88 with sigma of 0.02
 N17-H17B
 0.88 with sigma of 0.02
 N17-H17D
 0.88 with sigma of 0.02
2. Others
 Fixed Sof: N16A(0.5) O4WA(0.5) O5WA(0.5) O4W(0.5) O5W(0.5)
;
_shelx_res_checksum              4187
_olex2_submission_special_instructions 'No special instructions were received'