Synthetic Utility of Tetrabutylammonium Salts in Uranium Metallocene Chemistry
Webster, Christopher L.; Langeslay, Ryan R.; Ziller, Joseph W.; Evans, William J.; Organometallics 35 (2016) 520–; doi:10.1021/acs.organomet.5b00942

data_4088227
_publ_section_title
;
 Synthetic Utility of Tetrabutylammonium Salts in Uranium Metallocene
 Chemistry
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              520
_journal_paper_doi               10.1021/acs.organomet.5b00942
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C31 H51 N9 U'
_chemical_formula_weight         787.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9445(10)
_cell_length_b                   16.9108(9)
_cell_length_c                   19.7306(10)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.33
_cell_volume                     6321.0(6)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68683
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.916
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.172
_exptl_absorpt_correction_T_max  0.6246
_exptl_absorpt_correction_T_min  0.3916
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.141
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+6.0567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             6972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00942_si_008.cif
_cod_data_source_block           clw61
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088227
_shelx_estimated_absorpt_t_min   0.351
_shelx_estimated_absorpt_t_max   0.529
_shelxl_version_number           2013-3
_shelx_res_checksum              57220
_shelx_hkl_checksum              11469