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_7041464
_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_absolute_configuration rmad
_chemical_formula_moiety         'C64 H66 B2 N2 Nd2 Si2'
_chemical_formula_sum            'C64 H66 B2 N2 Nd2 Si2'
_chemical_formula_weight         1229.46
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5043(18)
_cell_length_b                   10.7865(8)
_cell_length_c                   27.740(2)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.750
_cell_measurement_theta_min      2.27
_cell_volume                     7032.9(9)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0681
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            62875
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.619
_diffrn_reflns_theta_min         1.468
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0873 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.8161.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;

;
_refine_diff_density_max         2.734
_refine_diff_density_min         -3.858
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         19092
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+14.2915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14406
_reflns_number_total             19092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04441g2.cif
_cod_data_source_block           4-Nd
_cod_depositor_comments
'Adding full bibliography for 7041456--7041465.cif.'
_cod_database_code               7041464
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.692
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(3) 0.48(3)
2. 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
3. Rigid bond restraints
 C32, C31
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C47 \\sim C48: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C21 \\sim C22: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C32 \\sim C33 \\sim C34: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C37) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C48)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C33) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C20(H20), C19(H19), C18(H18), C17(H17), C44(H44), C43(H43), C42(H42), C41(H41)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C47(H47A,H47B), C45(H45A,H45B)
5.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C48(H48A,H48B,H48C), C46(H46A,H46B,H46C), C14(H14A,H14B,H14C), C15(H15A,
 H15B,H15C)
5.d Aromatic/amide H refined with riding coordinates:
 C36(H36), C35(H35), C34(H34), C33(H33), C30(H30), C29(H29), C28(H28),
 C27(H27), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56)
;
_shelx_fab_checksum              26413
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'