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_7041462
_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         '2(C58 H76 B2 La2 N4 Si2), 1.5(C7 H8)'
_chemical_formula_sum            'C126.5 H164 B4 La4 N8 Si4'
_chemical_formula_weight         2507.89
_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   mixed
_audit_creation_date             2016-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-22 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                64.0720(10)
_cell_angle_beta                 67.2210(10)
_cell_angle_gamma                86.8250(10)
_cell_formula_units_Z            2
_cell_length_a                   18.7173(14)
_cell_length_b                   19.5181(14)
_cell_length_c                   21.7889(16)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.191
_cell_measurement_theta_min      2.272
_cell_volume                     6537.9(8)
_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      140.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.990
_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     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46821
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.136
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0647 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8965.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             2566
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;

;
_refine_diff_density_max         2.256
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1347
_refine_ls_number_reflns         25418
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0813P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18662
_reflns_number_total             25418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04441g2.cif
_cod_data_source_block           7-La
_cod_depositor_comments
'Adding full bibliography for 7041456--7041465.cif.'
_cod_original_formula_sum        'C126.50 H164 B4 La4 N8 Si4'
_cod_database_code               7041462
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H87 of C87, H13S of C13S, H88 of C88, H5S of C5S, H101
  of C101, H29 of C29, H63 of C63, H33 of C33, H27 of C27, H91 of C91, H3 of C3,
   H61 of C61, H1S of C1S, H10S of C10S, H85 of C85, H75 of C75, H93 of C93,
  H42 of C42, H12S of C12S, H92 of C92, H28 of C28, H2S of C2S, H4 of C4, H36
  of C36, H12 of C12, H30 of C30, H11S of C11S, H102 of C102, H11 of C11, H5 of
  C5, H34 of C34, H94 of C94, H43 of C43, H49 of C49, H14S of C14S, H3S of C3S,
  H64 of C64, H68 of C68, H70 of C70, H62 of C62, H86 of C86, H10 of C10, H76
  of C76, H9 of C9, H67 of C67, H77 of C77, H69 of C69, H20 of C20, H17 of C17,
  H78 of C78, H99 of C99, H35 of C35, H4S of C4S, H44 of C44, H19 of C19, H6 of
  C6, H18 of C18, H41 of C41, H100 of C100
 At 1.5 times of:
  All C(H,H,H) groups, H54 of C54
2. Restrained distances
 C8S-C9S = C45-C46
 1.53 with sigma of 0.01
 C8S-C10S = C8S-C14S
 2.4 with sigma of 0.01
 C49-H49 = C109-H109 = C114-H114 = C54-H54
 0.9 with sigma of 0.02
3. Rigid bond restraints
 N2, C45
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C45 \\sim C46: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C8S \\sim C9S \\sim C10S \\sim C11S \\sim C12S \\sim C13S \\sim C14S: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9S) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C8S) \\sim Ueq, Uanis(C9S) \\sim Ueq, Uanis(C10S) \\sim Ueq, Uanis(C11S)
\\sim Ueq, Uanis(C12S) \\sim Ueq, Uanis(C13S) \\sim Ueq, Uanis(C14S) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C8S(0.5) H8SA(0.5) H8SB(0.5) H8SC(0.5) C9S(0.5) C10S(0.5)
 H10S(0.5) C11S(0.5) H11S(0.5) C12S(0.5) H12S(0.5) C13S(0.5) H13S(0.5)
 C14S(0.5) H14S(0.5)
6.a Riding coordinates:
 C49(H49), C54(H54)
6.b Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C20(H20), C41(H41), C42(H42), C44(H44), C75(H75),
 C77(H77), C78(H78), C99(H99), C102(H102)
6.c Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C45(H45A,H45B), C47(H47A,H47B), C79(H79A,
 H79B), C81(H81A,H81B), C103(H10A,H10B), C105(H10F,H10G)
6.d Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C48(H48A,
 H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C72(H72A,H72B,
 H72C), C73(H73A,H73B,H73C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C),
 C104(H10C,H10D,H10E), C106(H10H,H10I,H10J), C107(H10K,H10L,H10M), C108(H10N,
 H10O,H10P), C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I),
 C116(H11J,H11K,H11L), C117(H11M,H11N,H11O), C118(H11P,H11Q,H11R), C7S(H7SA,
 H7SB,H7SC), C8S(H8SA,H8SB,H8SC)
6.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C19(H19), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35),
  C36(H36), C43(H43), C61(H61), C62(H62), C63(H63), C64(H64), C67(H67),
 C68(H68), C69(H69), C70(H70), C76(H76), C85(H85), C86(H86), C87(H87), C88(H88),
  C91(H91), C92(H92), C93(H93), C94(H94), C100(H100), C101(H101), C1S(H1S),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C10S(H10S), C11S(H11S), C12S(H12S),
 C13S(H13S), C14S(H14S)
6.f Fitted hexagon refined as free rotating group:
 C9S(C10S,C11S,C12S,C13S,C14S)
;
_shelx_fab_checksum              60063
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'