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_4087112
_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         'C44 H58 Cl2 O2 Si2 U'
_chemical_formula_sum            'C44 H58 Cl2 O2 Si2 U'
_chemical_formula_weight         984.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 116.312(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.144(13)
_cell_length_b                   9.884(5)
_cell_length_c                   24.028(13)
_cell_measurement_reflns_used    3595
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.08
_cell_measurement_theta_min      2.30
_cell_volume                     4927(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0977
_diffrn_reflns_av_unetI/netI     0.1063
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27400
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.637
_exptl_absorpt_coefficient_mu    3.481
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5511
_reflns_number_total             8909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00936_si_002.cif
_cod_data_source_block           compound10
_cod_database_code               4087112
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.543
_shelx_estimated_absorpt_t_max   0.623
_shelx_res_checksum              3068
_shelx_hkl_checksum              14751
_shelx_fab_checksum              14008