Synthesis and Structure of Silicon-Bridged Boratabenzene Fluorenyl Rare-Earth Metal Complexes
Wang, Chunhong; Xiang, Li; Leng, Xuebing; Chen, Yaofeng; Organometallics 35 (2016) 1995–; doi:10.1021/acs.organomet.6b00282

data_4088655
_publ_section_title
;
 Synthesis and Structure of Silicon-Bridged Boratabenzene Fluorenyl
 Rare-Earth Metal Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1995
_journal_paper_doi               10.1021/acs.organomet.6b00282
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C32 H44 B N O2 Si Sm'
_chemical_formula_weight         663.93
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.735(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5344(19)
_cell_length_b                   11.3397(13)
_cell_length_c                   17.0203(19)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      2.19
_cell_volume                     3039.6(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19382
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.503
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_T_max  0.6044
_exptl_absorpt_correction_T_min  0.5412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5941
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0359P)^2^+6.4402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5320
_reflns_number_total             5941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00282_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088655
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.541
_shelx_estimated_absorpt_t_max   0.604
_shelx_res_checksum              43208
_shelx_hkl_checksum              46895