Complexes of Th(IV) with neutral O-N-N-O hybrid ligands: a thermodynamic and crystallographic study.
Yang, Yanqiu; Lv, Lina; Liu, Yunnu; Chen, Baihua; Liu, Jun; Li, Xingliang; Luo, Shunzhong; Dalton transactions (Cambridge, England : 2003) 50 (2021) 705–714; doi:10.1039/d0dt03479g

data_7706028
_publ_section_title
;
 Complexes of Th(IV) with neutral O-N-N-O hybrid ligands: a thermodynamic
 and crystallographic study.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              705
_journal_page_last               714
_journal_paper_doi               10.1039/d0dt03479g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C32 H40 N8 O6 Th, 3(Cl O4), 2(C16 H18 N4 O2), 2(O)'
_chemical_formula_sum            'C64 H76 Cl3 N16 O24 Th'
_chemical_formula_weight         1791.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-20 deposited with the CCDC.	2020-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.528(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.5157(16)
_cell_length_b                   14.3850(14)
_cell_length_c                   17.7543(14)
_cell_measurement_reflns_used    3277
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.4240
_cell_measurement_theta_min      3.6260
_cell_volume                     4181.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  19.00   1.00   12.50    --  -14.81 -99.00  90.00   41
  2  \w      9.00  49.00   1.00   12.50    --   17.08 -99.00  30.00   40
  3  \w    -52.00  34.00   1.00   12.50    --   17.08 -38.00-180.00   86
  4  \w    -76.00 -16.00   1.00   12.50    --  -14.81 -19.00 -90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0235209000
_diffrn_orient_matrix_UB_12      0.0264322000
_diffrn_orient_matrix_UB_13      -0.0229575000
_diffrn_orient_matrix_UB_21      -0.0137406000
_diffrn_orient_matrix_UB_22      0.0415762000
_diffrn_orient_matrix_UB_23      0.0156656000
_diffrn_orient_matrix_UB_31      0.0337187000
_diffrn_orient_matrix_UB_32      -0.0015254000
_diffrn_orient_matrix_UB_33      0.0291630000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11137
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.856
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1810
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         11137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0777
_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^)+(0.1375P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6590
_reflns_number_total             11137
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9536\% 
 around [-0.71 0.00 0.71] (reciprocal) or [-0.76 0.00 0.65] (direct)
;
_cod_data_source_file            d0dt03479g1.cif
_cod_data_source_block           Th_TMBiPDA
_cod_depositor_comments
'Adding full bibliography for 7706028--7706029.cif.'
_cod_database_code               7706028
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3u1
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.548
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6061(17)
 0.3939(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3.a Rotating group:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C18(H18), C19(H19), C20(H20),
 C26(H26), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              66151
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.873
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2