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_4088663
_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         'C28 H36 B Gd I N O Si, C7 H8'
_chemical_formula_sum            'C35 H44 B Gd I N O Si'
_chemical_formula_weight         817.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5501(17)
_cell_length_b                   14.4106(13)
_cell_length_c                   13.5139(12)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.33
_cell_volume                     3410.0(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      132.65
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.977
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24295
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.830
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.7882.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.694
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         7290
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0287P)^2^+29.6879P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5959
_reflns_number_total             7290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00282_si_002.cif
_cod_data_source_block           10
_cod_database_code               4088663
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.622
_shelx_estimated_absorpt_t_min   0.530
_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. Rigid bond restraints
 C18, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C28 \\sim C27 \\sim C26: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(C10) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5)
4.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C28(H28A,H28B), C27(H27A,H27B), C26(H26A,
 H26B), C25(H25A,H25B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
4.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              10988
_shelx_hkl_checksum              4741
_olex2_submission_special_instructions 'No special instructions were received'