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_4088656
_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_moiety         'C32 H44 B N O2 Si Yb'
_chemical_formula_sum            'C32 H44 B N O2 Si Yb'
_chemical_formula_weight         686.62
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5521(15)
_cell_length_b                   11.1432(10)
_cell_length_c                   17.0640(15)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.547
_cell_measurement_theta_min      2.217
_cell_volume                     2993.0(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18936
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.498
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.194
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+2.7553P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5143
_reflns_number_total             5851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00282_si_002.cif
_cod_data_source_block           2
_cod_database_code               4088656
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C26(0.6) H26A(0.6) H26B(0.6) C27(0.6) H27A(0.6) H27B(0.6)
 C26'(0.4) H26C(0.4) H26D(0.4) C27'(0.4) H27C(0.4) H27D(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C26'(H26C,
 H26D), C27'(H27C,H27D), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              86844
_shelx_hkl_checksum              40634
_olex2_submission_special_instructions 'No special instructions were received'