Half-sandwich scandium boryl complexes bearing a silylene-linked cyclopentadienyl-amido ligand.
Wang, Baoli; Nishiura, Masayoshi; Cheng, Jianhua; Hou, Zhaomin; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14215–14218; doi:10.1039/c4dt01725k

data_7031685
_publ_section_title
;
 Half-sandwich scandium boryl complexes bearing a silylene-linked
 cyclopentadienyl-amido ligand.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14215
_journal_page_last               14218
_journal_paper_doi               10.1039/c4dt01725k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C43 H59 B Cl N3 Sc Si 1-,C12 H30 O6 Li 1+,C4 H10 O2,C6 H6'
_chemical_formula_sum            'C65 H105 B Cl Li N3 O8 Sc Si'
_chemical_formula_weight         1182.76
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                66.157(2)
_cell_angle_beta                 85.712(2)
_cell_angle_gamma                76.132(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3886(14)
_cell_length_b                   17.623(2)
_cell_length_c                   17.974(2)
_cell_measurement_reflns_used    258
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3483.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18555
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.239
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12104
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1910P)^2^+2.2850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2712
_refine_ls_wR_factor_ref         0.3139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7546
_reflns_number_total             12104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01725k2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7031681--7031685.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3483.7(7)
_cod_database_code               7031685
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-C68
 1.4 with sigma of 0.02
 O1-C55
 1.4 with sigma of 0.02
 O4B-C61
 1.4 with sigma of 0.02
 O4B-C60
 1.4 with sigma of 0.02
 O10-C78
 1.4 with sigma of 0.02
 C69-C71
 1.5 with sigma of 0.02
 O8-C70
 1.4 with sigma of 0.02
 O8-C71
 1.4 with sigma of 0.02
 O3-C59
 1.5 with sigma of 0.02
 O3-C58
 1.4 with sigma of 0.02
 C57-C58
 1.4 with sigma of 0.02
 C48-C49
 1.4 with sigma of 0.02
 C45-C46
 1.4 with sigma of 0.02
 C46-C47
 1.4 with sigma of 0.02
 O5-C72
 1.45 with sigma of 0.02
 O5-C72
 1.45 with sigma of 0.02
 C70-C73
 1.53 with sigma of 0.02
 O4-C73
 1.4 with sigma of 0.02
 Li1-C71
 2.4 with sigma of 0.02
 O3-Li1 \\sim O7-Li1
 with sigma of 0.02
 O4B-C60 \\sim O4A-C61
 with sigma of 0.02
 O4B-C62 \\sim O4A-C62
 with sigma of 0.02
 O4A-Li1 \\sim O4B-Li1
 with sigma of 0.02
 O5-Li1 \\sim O6-Li1
 with sigma of 0.02
 O5-C72 \\sim O4-C54B
 with sigma of 0.02
 O1-C54A \\sim O4-C54B
 with sigma of 0.02
 O1-Li1 \\sim O4-Li1 \\sim O8-Li1 \\sim O5-Li1 \\sim O4B-Li1 \\sim O4A-Li1
\\sim O3-Li1 \\sim O7-Li1 \\sim O6-
 Li1 \\sim O5-Li1
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(C68) = Uiso(C69) = Uiso(C71)
Uanis(C45) = Uanis(C47) = Uanis(C48)
Uiso(O1) = Uiso(O4)
Uiso(O5) = Uiso(O8)
Uiso(C73) = Uiso(C54A)
4. Rigid body (RIGU) restrains
 C44, C45, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.5) O5(0.5) O7(0.5) O8(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 H62C(0.5) H62D(0.5) H62A(0.5) H62B(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
 H63D(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C68(0.5) H68A(0.5) H68B(0.5)
 H68C(0.5) C69(0.5) H69A(0.5) H69B(0.5) C71(0.5) H71A(0.5) H71B(0.5) O3(0.5)
 O6(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C58(0.5) H58A(0.5) H58B(0.5)
 C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) O4B(0.5) C54B(0.5) H54A(0.5) H54B(0.5)
 H54C(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5)
 H61C(0.5) C53(0.7) H53A(0.7) H53B(0.7) H53C(0.7) C78(0.3) H78A(0.3) H78B(0.3)
 H78C(0.3) O4A(0.5) O4(0.5) O5(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5)
 C54A(0.5) H54D(0.5) H54E(0.5) H54F(0.5) C73(0.5) H73A(0.5) H73B(0.5)
6.a Riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C26(H26), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42), C43(H43A,H43B,H43C), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C78(H78A,H78B,H78C)
6.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C62(H62C,H62D), C62(H62A,
 H62B), C63(H63A,H63B), C63(H63C,H63D), C69(H69A,H69B), C71(H71A,H71B),
 C58(H58A,H58B), C73(H73A,H73B)
6.c Me refined with riding coordinates:
 C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C67(H67A,H67B,H67C), C59(H59A,H59B,
 H59C), C54B(H54A,H54B,H54C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C72(H72A,H72B,H72C), C54A(H54D,H54E,H54F)
6.d Aromatic/amide H refined with riding coordinates:
 C46(H46), C45(H45), C44(H44), C48(H48), C47(H47), C49(H49)
;
_olex2_submission_special_instructions 'No special instructions were received'