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_4086231
_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_absolute_configuration ad
_chemical_formula_sum            'C38 H40 B3 La N2'
_chemical_formula_weight         696.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.026(3)
_cell_length_b                   8.9614(10)
_cell_length_c                   15.8076(18)
_cell_measurement_reflns_used    7518
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      2.43
_cell_volume                     3403.5(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0629
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21225
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.129
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.363
_refine_diff_density_min         -3.073
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
; 
 Flack x determined using 2135 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.049(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.6174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0804
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                5382
_reflns_number_total             6622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00262_si_002.cif
_cod_data_source_block           dm11358
_cod_database_code               4086231
_shelx_estimated_absorpt_t_min   0.699
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2014-3
_shelx_res_checksum              97978
_shelx_hkl_checksum              2567