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_4088657
_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            'C74.5 H84 B2 N2 Si2 Yb2'
_chemical_formula_weight         1431.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 114.1480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.1436(15)
_cell_length_b                   36.891(3)
_cell_length_c                   20.4285(14)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.38
_cell_volume                     14540.0(19)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58127
_diffrn_reflns_point_group_measured_fraction_full 0.842
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         1.104
_exptl_absorpt_coefficient_mu    2.629
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
;
_refine_diff_density_max         1.932
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
; 
 Flack x determined using 7984 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.684(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1474
_refine_ls_number_reflns         27467
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.642
_reflns_Friedel_fraction_full    0.688
_reflns_Friedel_fraction_max     0.638
_reflns_number_gt                22861
_reflns_number_total             27467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00282_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;

2020-05-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C149 H168 B4 N4 Si4 Yb4'
_cod_original_formula_weight         2862.62
_cod_original_formula_units_Z            4
_cod_original_cell_volume        14540.2(18)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4088657
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.858
_shelxl_version_number           2013-4
_shelx_res_checksum              38428
_shelx_hkl_checksum              40983