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_4087109
_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         'C43 H70 N2 Si2 U'
_chemical_formula_sum            'C43 H70 N2 Si2 U'
_chemical_formula_weight         909.22
_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                 106.680(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.921(13)
_cell_length_b                   15.613(14)
_cell_length_c                   19.435(18)
_cell_measurement_reflns_used    3568
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.77
_cell_measurement_theta_min      2.19
_cell_volume                     4337(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.982
_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  0.1202
_diffrn_reflns_av_unetI/netI     0.1487
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26776
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         1.527
_exptl_absorpt_coefficient_mu    3.827
_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            orange
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.866
_refine_diff_density_min         -4.152
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         9787
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0827P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5968
_reflns_number_total             9787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00936_si_002.cif
_cod_data_source_block           compound7
_cod_database_code               4087109
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.515
_shelx_estimated_absorpt_t_max   0.701
_shelx_res_checksum              88999
_shelx_hkl_checksum              93086