Experimental and Computational Studies of a Uranium Metallacyclocumulene
Zhang, Lei; Fang, Bo; Hou, Guohua; Zi, Guofu; Ding, Wanjian; Walter, Marc D.; Organometallics 36 (2017) 898–; doi:10.1021/acs.organomet.6b00936

data_4087110
_publ_section_title
;
 Experimental and Computational Studies of a Uranium Metallacyclocumulene
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              898
_journal_paper_doi               10.1021/acs.organomet.6b00936
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C37 H58 N2 Si2 U'
_chemical_formula_sum            'C37 H58 N2 Si2 U'
_chemical_formula_weight         825.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                103.281(12)
_cell_angle_beta                 92.099(13)
_cell_angle_gamma                100.821(13)
_cell_formula_units_Z            4
_cell_length_a                   12.006(9)
_cell_length_b                   16.997(13)
_cell_length_c                   18.691(14)
_cell_measurement_reflns_used    5282
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.31
_cell_volume                     3633(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker 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  0.0762
_diffrn_reflns_av_unetI/netI     0.1313
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20516
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.470
_exptl_absorpt_coefficient_mu    4.560
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.242
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         13035
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9465
_reflns_number_total             13035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00936_si_002.cif
_cod_data_source_block           compound8
_cod_database_code               4087110
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.462
_shelx_estimated_absorpt_t_max   0.548
_shelx_res_checksum              68216
_shelx_hkl_checksum              92987