New supporting ligands in actinide chemistry: tetramethyltetraazaannulene complexes with thorium and uranium
Hohloch, Stephan; Garner, Mary E.; Parker, Bernard F.; Arnold, John; Dalton Trans.  (2017) –; doi:10.1039/C7DT02682J

data_7044355
_publ_section_title
;
 New supporting ligands in actinide chemistry: tetramethyltetraazaannulene
 complexes with thorium and uranium
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02682J
_journal_year                    2017
_chemical_formula_sum            'C30 H38 Cl2 N4 O2 Th'
_chemical_formula_weight         789.58
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-12 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   12.5806(4)
_cell_length_c                   26.4577(9)
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_cell_measurement_theta_min      1.539
_cell_volume                     3031.10(17)
_computing_cell_refinement       'Bruker ApexII suite, 2008'
_computing_data_collection       'Bruker ApexII suite, 2008'
_computing_data_reduction        'Bruker ApexII suite, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51711
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.446
_diffrn_reflns_theta_min         1.539
_exptl_absorpt_coefficient_mu    5.129
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.086
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_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.394(7)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0170P)^2^+2.7160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0476
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_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5493
_reflns_number_total             5579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02682j2.cif
_cod_data_source_block           shelx
_cod_database_code               7044355
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.233
_shelx_estimated_absorpt_t_max   0.904
_shelx_res_checksum              86470