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_7707599
_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 H2 N4 O3 S4 U, 2(C8 H20 N), H2 O'
_chemical_formula_sum            'C20 H44 N6 O4 S4 U'
_chemical_formula_weight         798.88
_chemical_name_common            (C8H20N)2[UO2(NCS)4(H2O)](H2O)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.443(3)
_cell_length_b                   7.8475(8)
_cell_length_c                   13.5033(12)
_cell_measurement_reflns_used    7651
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.302
_cell_measurement_theta_min      2.675
_cell_volume                     3226.0(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_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  0.0660
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28988
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.387
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.323
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5811
_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            'intense yellow'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 2211 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6550
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0308
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                5408
_reflns_number_total             6550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01464a4.cif
_cod_data_source_block           NMB_Compound_5
_cod_depositor_comments
'Adding full bibliography for 7707598--7707604.cif.'
_cod_original_cell_volume        3226.0(6)
_cod_database_code               7707599
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.441
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H3b-O3 = H3b-H3a
 0.82 with sigma of 0.02
 H3a-O3 = H3a-H3b
 0.82 with sigma of 0.02
 H4b-O4
 0.82 with sigma of 0.02
 H4a-O4
 0.82 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C7(H7a,H7b), C12(H12a,H12b), C20(H20a,H20b), C30(H30a,H30b),
 C32(H32a,H32b), C40(H40a,H40b), C41(H41a,H41b)
3.b Me refined with riding coordinates:
 C10(H10a,H10b,H10c), C13(H13a,H13b,H13c), C11(H11a,H11b,H11c), C8(H8a,H8b,
 H8c), C60(H60a,H60b,H60c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C70(H70a,
 H70b,H70c)
;
_shelx_res_checksum              43509
_shelx_hkl_checksum              18570
_olex2_submission_special_instructions 'No special instructions were received'