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_7041461
_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         'C62 H68 B2 La2 N4 Si2, 3(C6 H6)'
_chemical_formula_sum            'C80 H86 B2 La2 N4 Si2'
_chemical_formula_weight         1459.14
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2016-11-22 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                73.746(3)
_cell_angle_beta                 85.409(3)
_cell_angle_gamma                89.834(3)
_cell_formula_units_Z            1
_cell_length_a                   10.7103(19)
_cell_length_b                   11.678(2)
_cell_length_c                   14.604(3)
_cell_measurement_reflns_used    5717
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.697
_cell_measurement_theta_min      2.30
_cell_volume                     1747.6(6)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.15
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11432
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.457
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0954 before and 0.0554 after correction.
The Ratio of minimum to maximum transmission is 0.6779.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       plate
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.532
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6397
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0701P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5425
_reflns_number_total             6397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04441g2.cif
_cod_data_source_block           mo_dm13408_0m
_cod_depositor_comments
'Adding full bibliography for 7041456--7041465.cif.'
_cod_original_cell_volume        1747.5(5)
_cod_database_code               7041461
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.731
_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. Restrained distances
 N1-C25 = N1-C25'
 1.34 with sigma of 0.01
 C25-C26 = C25'-C26'
 1.5 with sigma of 0.01
 C32-C37
 1.39 with sigma of 0.01
 C25'-C27' = C25'-C31'
 2.56 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C25'
\\sim C26' \\sim C27' \\sim C28' \\sim C29' \\sim C30' \\sim C31': within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C25(0.5) H25(0.5) C26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5)
 C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C25'(0.5) H25'(0.5)
 C26'(0.5) C27'(0.5) H27'(0.5) C28'(0.5) H28'(0.5) C29'(0.5) H29'(0.5)
 C30'(0.5) H30'(0.5) C31'(0.5) H31'(0.5)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B)
5.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C)
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),
 C16(H16), C20(H20), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C25'(H25'), C27'(H27'), C28'(H28'), C29'(H29'), C30'(H30'), C31'(H31'),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
  C40(H40)
5.e Fitted hexagon refined as free rotating group:
 C26(C27,C28,C29,C30,C31), C26'(C27',C28',C29',C30',C31'), C32(C33,C34,C35,C36,
 C37)
;
_shelx_res_checksum              47293
_olex2_submission_special_instructions 'No special instructions were received'