Tris(boratabenzene) Lanthanum Complexes: Synthesis, Structure, and Reactivity
Wang, Chunhong; Leng, Xuebing; Chen, Yaofeng; Organometallics 34 (2015) 3216–; doi:10.1021/acs.organomet.5b00262

data_4086230
_publ_section_title
;
 Tris(boratabenzene) Lanthanum Complexes: Synthesis, Structure, and
 Reactivity
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3216
_journal_paper_doi               10.1021/acs.organomet.5b00262
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C22 H32 B3 La N2'
_chemical_formula_weight         495.83
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 93.0610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.770(3)
_cell_length_b                   8.6243(7)
_cell_length_c                   16.5042(13)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      31.56
_cell_measurement_theta_min      2.47
_cell_volume                     4515.6(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 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0187
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17912
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.284
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4896
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+5.8951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4488
_reflns_number_total             4896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00262_si_002.cif
_cod_data_source_block           mo_dm1173_0m
_cod_original_cell_volume        4515.6(6)
_cod_database_code               4086230
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.764
_shelxl_version_number           2014-3
_shelx_res_checksum              45278
_shelx_hkl_checksum              58222