Bimetallic uranyl/cobalt(II) isothiocyanates: structure, property and spectroscopic analysis of homo- and heterometallic phases.
Byrne, Nicole M.; Schofield, Mark H.; Nicholas, Aaron D.; Cahill, Christopher L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9158–9172; doi:10.1039/d1dt01464a

data_7707604
_publ_section_title
;
 Bimetallic uranyl/cobalt(II) isothiocyanates: structure, property and
 spectroscopic analysis of homo- and heterometallic phases.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9158
_journal_page_last               9172
_journal_paper_doi               10.1039/d1dt01464a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C4 Co N4 S4, 2(C4 H12 N)'
_chemical_formula_sum            'C12 H24 Co N6 S4'
_chemical_formula_weight         439.54
_chemical_name_common            '[Co(NCS)4](C4H12N)2'
_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     direct
_audit_creation_date             2021-04-14
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-16 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                95.465(5)
_cell_angle_beta                 90.187(6)
_cell_angle_gamma                114.197(5)
_cell_formula_units_Z            6
_cell_length_a                   11.1036(18)
_cell_length_b                   13.2845(18)
_cell_length_c                   24.380(4)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.678
_cell_measurement_theta_min      2.159
_cell_volume                     3261.8(9)
_computing_cell_refinement       'APEX3 v2019.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.12'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXT 2014/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83049
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.730
_diffrn_reflns_theta_min         1.965
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'clear intense blue'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         12389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0364
_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/[\s^2^(Fo^2^)+(0.0216P)^2^+4.5242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11604
_reflns_number_total             12389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01464a4.cif
_cod_data_source_block           NMB_Compound_2
_cod_depositor_comments
'Adding full bibliography for 7707598--7707604.cif.'
_cod_original_cell_volume        3261.8(8)
_cod_database_code               7707604
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.667
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7687(7)
 0.2313(7)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C32(H32A,H32B,H32C), C14(H14A,H14B,
 H14C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C23(H23A,
 H23B,H23C), C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C35(H35A,H35B,H35C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              58306
_shelx_hkl_checksum              66463
_olex2_submission_special_instructions 'No special instructions were received'