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_4088665
_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_absolute_configuration rmad
_chemical_formula_moiety         'C37 H48 B Gd N2 O Si'
_chemical_formula_sum            'C37 H48 B Gd N2 O Si'
_chemical_formula_weight         732.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.482(3)
_cell_length_b                   16.964(5)
_cell_length_c                   21.258(7)
_cell_measurement_reflns_used    3515
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      30.443
_cell_measurement_theta_min      2.342
_cell_volume                     3419.4(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0760
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18761
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         1.536
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.005
_exptl_absorpt_correction_T_max  0.8560
_exptl_absorpt_correction_T_min  0.5845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1090 before and 0.0753 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1494 before and 0.0985 after correction.
 The Ratio of minimum to maximum transmission is 0.45.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 38333 reflections, Rint = 0.1299
 (19673 with I > 3sig(I), Rint = 0.1155)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.635
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+109.3978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.1908
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5844
_reflns_number_total             6059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00282_si_002.cif
_cod_data_source_block           13a
_cod_original_cell_volume        3419.5(18)
_cod_database_code               4088665
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.584
_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-C21 = N1-C24'
 1.48 with sigma of 0.01
 H21B-H23A
 1.9 with sigma of 0.01
3. Rigid bond restraints
 O1, C34
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C36 \\sim C37: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C20) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C24') \\sim Ueq, Uanis(C25') \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(B1)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C24'(0.5) H24D(0.5) H24E(0.5) C25'(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C1(H1), C4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C21(H21A,H21B), C24'(H24D,H24E), C25(H25D,H25E), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
6.c Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C22(H22A,H22B,
 H22C), C25'(H25A,H25B,H25C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
6.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C13(H13), C12(H12),
 C11(H11), C5(H5), C30(H30), C29(H29), C28(H28), C27(H27)
;
_shelx_res_checksum              17780
_shelx_hkl_checksum              39638
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'