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_4132313
_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         'C20 H31 B Cl Mo N6 O2 P, 2(C4 H8 O)'
_chemical_formula_sum            'C28.04 H47 B Cl1.02 Mo N6 O4.04 P'
_chemical_formula_weight         706.55
_chemical_name_systematic        PG-211
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.068(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9014(13)
_cell_length_b                   11.8934(12)
_cell_length_c                   20.261(2)
_cell_measurement_reflns_used    9584
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.64
_cell_volume                     3349.3(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            92324
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.457
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.8499
_exptl_absorpt_correction_T_min  0.7297
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sadabs (2014/2, Bruker AXS Gmbh Karlsruhe)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             1475
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.247
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8066
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0603P)^2^+10.1303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6661
_reflns_number_total             8066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02902_si_002.cif
_cod_data_source_block           2505f
_cod_database_code               4132313
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.729
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H) groups,
  All C(H,H,H,H) groups
2. Shared sites
{C19, C19T}
{C19S, C20T}
{C20, C20S}
{O1, O1T}
{O1S, O2T}
{O2, O2S}
{Mo, MoS, MoT}
3. Restrained distances
 C20-O2 = C20-O2S
 1.19 with sigma of 0.001
 Mo-ClS \\sim Mo-ClT \\sim Mo-Cl
 with sigma of 0.001
 Mo-C19 \\sim Mo-C19S \\sim Mo-C19T
 with sigma of 0.001
 C22-C23 \\sim C22-C23S \\sim C23-C24 \\sim C23S-C24
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Cl \\sim ClS \\sim ClT: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(Cl) \\sim Ueq, Uanis(ClS) \\sim Ueq, Uanis(ClT) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C23S) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C19) = Uanis(C19T)
Uanis(C19S) = Uanis(C20T)
Uanis(C20) = Uanis(C20S)
Uanis(O1) = Uanis(O1T)
Uanis(O1S) = Uanis(O2T)
Uanis(O2) = Uanis(O2S)
Uanis(Mo) = Uanis(MoS) = Uanis(MoT)
5. Others
 1*[Sof(Mo)+Sof(Cl)+Sof(O1)+Sof(O2)+Sof(C19)+Sof(C20)]+1*[Sof(MoS)+Sof(ClS)+
 Sof(O1S)+Sof(O2S)+Sof(C19S)+Sof(C20S)]+1*[Sof(MoT)+Sof(ClT)+Sof(O1T)+Sof(O2T)+
 Sof(C19T)+Sof(C20T)]=1 with esd of 0.0001
 Sof(Mo)=Sof(Cl)=Sof(O1)=Sof(O2)=Sof(C19)=Sof(C20)=FVAR(1)
 Sof(MoS)=Sof(ClS)=Sof(O1S)=Sof(O2S)=Sof(C19S)=Sof(C20S)=FVAR(2)
 Sof(MoT)=Sof(ClT)=Sof(O1T)=Sof(O2T)=Sof(C19T)=Sof(C20T)=FVAR(3)
 Sof(H22C)=Sof(H22D)=Sof(C23S)=Sof(H23C)=Sof(H23D)=Sof(H24C)=Sof(H24D)=1-FVAR(4)
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H24A)=Sof(H24B)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C22(H22C,H22D), C23(H23A,H23B), C23S(H23C,
 H23D), C24(H24A,H24B), C24(H24C,H24D), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              37097
_shelx_hkl_checksum              67536
_olex2_submission_special_instructions 'No special instructions were received'