Rare-earth metal hydrides supported by silicon-bridged boratabenzene fluorenyl ligands: synthesis, structure and reactivity.
Wang, Chunhong; Xiang, Li; Leng, Xuebing; Chen, Yaofeng; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1218–1227; doi:10.1039/c6dt04441g

data_7041465
_publ_section_title
;
 Rare-earth metal hydrides supported by silicon-bridged boratabenzene
 fluorenyl ligands: synthesis, structure and reactivity.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1218
_journal_page_last               1227
_journal_paper_doi               10.1039/c6dt04441g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C28 H37 B La N O Si'
_chemical_formula_sum            'C28 H37 B La N O Si'
_chemical_formula_weight         581.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-11-22 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.818(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.463(3)
_cell_length_b                   17.602(3)
_cell_length_c                   19.082(3)
_cell_measurement_reflns_used    2766
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.783
_cell_measurement_theta_min      2.31
_cell_volume                     5365.9(16)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.15
_diffrn_measured_fraction_theta_full 0.996
_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  0.1145
_diffrn_reflns_av_unetI/netI     0.1342
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26126
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.510
_diffrn_reflns_theta_min         1.721
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0915 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission is 0.8015.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.433
_refine_diff_density_min         -2.001
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         8162
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4831
_reflns_number_total             8162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04441g2.cif
_cod_data_source_block           3-La
_cod_depositor_comments
'Adding full bibliography for 7041456--7041465.cif.'
_cod_original_cell_volume        5366.1(16)
_cod_database_code               7041465
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.733
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All La(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C23-C24 = C23'-C24'
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C23 \\sim C24 \\sim C23' \\sim C24': within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
C22 \\sim C21: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
4. Others
 Fixed Sof: C23(0.5) H23A(0.5) H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5) C23'(0.5) H23C(0.5) H23D(0.5) C24'(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
5.a Riding coordinates:
 La1(H,HA)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C23'(H23C,H23D), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B)
5.c Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C24'(H24D,H24E,H24F)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C20(H20)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'