Linearly Two-Coordinated Silicon: Transition Metal Complexes with the Functional Groups M≡Si-M and M═Si═M.
Ghana, Priyabrata; Arz, Marius I.; Chakraborty, Uttam; Schnakenburg, Gregor; Filippou, Alexander C.; Journal of the American Chemical Society 140 (2018) 7187–7198; doi:10.1021/jacs.8b02902

data_4132319
_publ_section_title
;
 Linearly Two-Coordinated Silicon: Transition Metal Complexes with the
 Functional Groups M\\tb Si-M and M&#x2550;Si&#x2550;M.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7187
_journal_page_last               7198
_journal_paper_doi               10.1021/jacs.8b02902
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '2(C41 H71 B Mo N6 O2 Si5), 3(C6 H6)'
_chemical_formula_sum            'C100 H160 B2 Mo2 N12 O4 Si10'
_chemical_formula_weight         2088.79
_chemical_name_systematic        P.G.-451
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4975)
;
_cell_angle_alpha                103.244(2)
_cell_angle_beta                 93.358(2)
_cell_angle_gamma                93.082(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3366(8)
_cell_length_b                   16.7705(11)
_cell_length_c                   26.6283(18)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.36
_cell_volume                     5773.5(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8-KappaApex-II'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            68029
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.403
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0870 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.8735.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       plate
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         24773
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0355P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15421
_reflns_number_total             24773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02902_si_002.cif
_cod_data_source_block           3875f
_cod_database_code               4132319
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Si3, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 Si3, C12
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C13 \\sim C12 \\sim Si3 \\sim C11: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
4. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=1-FVAR(1)
 Sof(C15')=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16')=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17')=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C18(H18), B(H), C7'(H7'), C18'(H18'), B'(H')
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C28(H28), C33(H33), C38(H38), C3'(H3'), C5'(H5'), C28'(H28'),
 C33'(H33'), C38'(H38'), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C47(H47), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10D,H10E,H10F), C11(H11D,H11E,H11F),
 C12(H12D,H12E,H12F), C13(H13D,H13E,H13F), C15(H15D,H15E,H15F), C16(H16D,H16E,
 H16F), C17(H17D,H17E,H17F), C19(H19D,H19E,H19F), C20(H20D,H20E,H20F), C21(H21D,
 H21E,H21F), C22(H22D,H22E,H22F), C23(H23D,H23E,H23F), C24(H24D,H24E,H24F),
 C30(H30D,H30E,H30F), C31(H31D,H31E,H31F), C35(H35D,H35E,H35F), C36(H36D,H36E,
 H36F), C40(H40D,H40E,H40F), C41(H41D,H41E,H41F), C8'(H8'A,H8'B,H8'C), C9'(H9'A,
 H9'B,H9'C), C10'(H10A,H10B,H10C), C11'(H11A,H11B,H11C), C12'(H12A,H12B,H12C),
 C13'(H13A,H13B,H13C), C15'(H15A,H15B,H15C), C16'(H16A,H16B,H16C), C17'(H17A,
 H17B,H17C), C19'(H19A,H19B,H19C), C20'(H20A,H20B,H20C), C21'(H21A,H21B,H21C),
 C22'(H22A,H22B,H22C), C23'(H23A,H23B,H23C), C24'(H24A,H24B,H24C), C30'(H30A,
 H30B,H30C), C31'(H31A,H31B,H31C), C35'(H35A,H35B,H35C), C36'(H36A,H36B,H36C),
 C40'(H40A,H40B,H40C), C41'(H41A,H41B,H41C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,
 H1BC), C1C(H1CA,H1CB,H1CC)
;
_shelx_res_checksum              93525
_shelx_hkl_checksum              42232
_olex2_submission_special_instructions 'No special instructions were received'