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_4132314
_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         'C28 H51 B Mo N6 Na O6 P, 0.5(C4 H10 O2)'
_chemical_formula_sum            'C30 H56 B Mo N6 Na O7 P'
_chemical_formula_weight         773.51
_chemical_name_systematic        PG-164
_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
_audit_creation_date             2018-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.912(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2762(7)
_cell_length_b                   14.4377(4)
_cell_length_c                   16.8995(7)
_cell_measurement_reflns_used    11585
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.80
_cell_volume                     3823.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31781
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.822
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.9868
_exptl_absorpt_correction_T_min  0.9241
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.135
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9212
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0785P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6493
_reflns_number_total             9212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02902_si_002.cif
_cod_data_source_block           2352
_cod_database_code               4132314
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.924
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, {H10A,H10B,H10C} of C10, {H9A,H9B,H9C} of C9, {H5A,H5B,
  H5C} of C5, {H4A,H4B,H4C} of C4, {H14A,H14B,H14C} of C14, {H15A,H15B,H15C} of
  C15, {H16A,H16B,H16C} of C16, {H17A,H17B,H17C} of C17, {H18A,H18B,H18C} of
  C18, {H23A,H23B,H23C} of C23, {H24A,H24B,H24C} of C24, All C(H) groups, All
  C(H,H) groups
 At 1.5 times of:
  {H27A,H27B,H27C} of C27, {H28A,H28B,H28C} of C28, {H31A,H31B,H31C} of C31,
  {H32A,H32B,H32C} of C32
2. Rigid bond restraints
 O2, C20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Mo, C19
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Mo, C20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Na \\sim O3 \\sim O4 \\sim C21 \\sim C22 \\sim C23: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
Uanis(C31) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Others
 Fixed Sof: O7(0.5) O8(0.5) C29(0.5) H29A(0.5) H29B(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C29(H29A,
 H29B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12)
5.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), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              40596
_shelx_hkl_checksum              72522
_olex2_submission_special_instructions 'No special instructions were received'