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_2243976
_publ_section_title
;
 Crystal structures of metallocene complexes with uranium--germanium bonds
;
_journal_coeditor_code           VM2256
_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 H I]'
_chemical_formula_moiety         'C36 H37 F12 Ge I U'
_chemical_formula_sum            'C36 H37 F12 Ge I U'
_chemical_formula_weight         1135.17
_chemical_name_systematic
Bis[3,5-bis(trifluoromethyl)phenyl-2\k<i>C</i>^1^](hydrido-2\k<i>H</i>)(iodido-1\k<i>I</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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.727(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.647(2)
_cell_length_b                   21.123(2)
_cell_length_c                   16.8132(18)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.32
_cell_volume                     7905.2(13)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker VENTURE CMOS area detector'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            103146
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         2.054
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.714
_exptl_absorpt_correction_T_max  0.5629
_exptl_absorpt_correction_T_min  0.1364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>AXScale</i>; Bruker, 2015
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.625
_exptl_crystal_size_min          0.525
_refine_diff_density_max         2.634
_refine_diff_density_min         -1.998
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9105
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0386P)^2^+173.3198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                7700
_reflns_number_total             9105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2256sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        7905.1(14)
_cod_database_code               2243976
_shelx_estimated_absorpt_t_min   0.121
_shelx_estimated_absorpt_t_max   0.153
_shelx_hkl_checksum              56015
_shelx_res_checksum              2288
_cod_database_fobs_code 2243976