Crystal structures of metallocene complexes with uranium–germanium bonds
Tarlton, Michael L.; Kelley, Steven P.; Walensky, Justin R.; Acta Crystallographica Section E 77 (2021) 1258–1262; doi:10.1107/S2056989021011269

data_2243977
_publ_section_title
;
 Crystal structures of metallocene complexes with uranium--germanium bonds
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1258
_journal_page_last               1262
_journal_paper_doi               10.1107/S2056989021011269
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Ge U (C10 H15)2 (C8 H3 F6)2 F H]'
_chemical_formula_moiety         'C37 H39 F13 Ge U'
_chemical_formula_sum            'C37 H39 F13 Ge U'
_chemical_formula_weight         1041.30
_chemical_name_systematic
Bis[3,5-bis(trifluoromethyl)phenyl-2\k<i>C</i>^1^](fluorido-1\k<i>I</i>)(hydrido-2\k<i>H</i>)bis[1,1(\h^5^)-pentamethylcyclopentadienyl]germaniumuranium(<i>Ge</i>---<i>U</i>)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 95.028(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.160(3)
_cell_length_b                   13.5237(11)
_cell_length_c                   16.2986(13)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.34
_cell_volume                     7500.5(11)
_computing_cell_refinement
;
APEX3 and SAINT Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
APEX3 and SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65643
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.455
_diffrn_reflns_theta_min         1.620
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.5010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_description       prism
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.680
_refine_diff_density_min         -0.782
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0441P)^2^+21.6495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                5563
_reflns_number_total             7720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2256sup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        7500.4(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2243977
_shelx_estimated_absorpt_t_min   0.624
_shelx_estimated_absorpt_t_max   0.681
_shelx_hkl_checksum              90146
_shelx_res_checksum              55806
_cod_database_fobs_code 2243977