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_4132316
_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(C37 H53 B2 Mo2 N12 O4 P Si), C5 H12'
_chemical_formula_sum            'C79 H118 B4 Mo4 N24 O8 P2 Si2'
_chemical_formula_weight         2077.09
_chemical_name_systematic        PG-167.3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 104.783(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9565(16)
_cell_length_b                   25.378(4)
_cell_length_c                   16.080(2)
_cell_measurement_reflns_used    2924
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.62
_cell_volume                     4717.7(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10059
_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         25.247
_diffrn_reflns_theta_min         2.449
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.8661
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.895
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         10059
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0070P)^2^+34.7860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8436
_reflns_number_total             10059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02902_si_002.cif
_cod_data_source_block           2219
_cod_original_cell_volume        4717.9(12)
_cod_database_code               4132316
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8618(13)
 0.1382(13)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, {H35A,H35B,H35C} of C35, {H34A,H34B,H34C} of C34, {H4A,H4B,
  H4C} of C4, {H5A,H5B,H5C} of C5, {H9A,H9B,H9C} of C9, {H10A,H10B,H10C} of C10,
   {H14A,H14B,H14C} of C14, {H15A,H15B,H15C} of C15, {H21A,H21B,H21C} of C21,
  {H22A,H22B,H22C} of C22, {H26A,H26B,H26C} of C26, {H27A,H27B,H27C} of C27,
  {H31A,H31B,H31C} of C31, {H32A,H32B,H32C} of C32, {H33A,H33B,H33C} of C33,
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  {H42A,H42B,H42C} of C42, {H38A,H38B,H38C} of C38
3. Restrained distances
 B1-H1
 1.17 with sigma of 0.002
 B2-H2A
 1.17 with sigma of 0.002
4. Rigid bond restraints
 Mo2, Si
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
6. Others
 Fixed Sof: C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5)
 H42A(0.5) H42B(0.5) H42C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C19(H19), C24(H24), C29(H29)
7.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), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C38(H38A,H38B,H38C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              48627
_shelx_hkl_checksum              78032
_olex2_submission_special_instructions 'No special instructions were received'