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_7707598
_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         'C5 N5 O2 S5 U, 3(C4 H12 N)'
_chemical_formula_sum            'C17 H36 N8 O2 S5 U'
_chemical_formula_weight         782.87
_chemical_name_common            '[UO2(NCS)5](C4H12N)3'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 97.732(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3772(14)
_cell_length_b                   9.2787(8)
_cell_length_c                   20.3648(17)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.227
_cell_measurement_theta_min      2.229
_cell_volume                     3066.5(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0867
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            115788
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.661
_exptl_absorpt_correction_T_max  0.7185
_exptl_absorpt_correction_T_min  0.6291
_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 yellow'
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+4.2211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5360
_reflns_number_total             6288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01464a4.cif
_cod_data_source_block           NMB_Compound_1
_cod_depositor_comments
'Adding full bibliography for 7707598--7707604.cif.'
_cod_database_code               7707598
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.654
_shelx_estimated_absorpt_t_min   0.334
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
S5 \\sim S2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Sof(S3)=1-FVAR(1)
 Sof(S3A)=FVAR(1)
4.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
  C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C14(H14A,H14B,
 H14C)
;
_shelx_res_checksum              42337
_shelx_hkl_checksum              52395
_olex2_submission_special_instructions 'No special instructions were received'