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_4132317
_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 H32 B Mo N6 O2 P, C6 H6'
_chemical_formula_sum            'C26 H38 B Mo N6 O2 P'
_chemical_formula_weight         604.36
_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_Int_Tables_number      2
_audit_creation_date             2014-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                109.005(2)
_cell_angle_beta                 95.885(2)
_cell_angle_gamma                95.334(2)
_cell_formula_units_Z            4
_cell_length_a                   13.5471(4)
_cell_length_b                   14.2491(4)
_cell_length_c                   16.2990(5)
_cell_measurement_reflns_used    21234
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.67
_cell_volume                     2932.26(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.9760
_diffrn_measured_fraction_theta_max 0.9738
_diffrn_measurement_details      ' 185 frames, detector distance = 100 mm'
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25134
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.67
_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    0.535
_exptl_absorpt_correction_T_max  0.8581
_exptl_absorpt_correction_T_min  0.7161
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Xred (SOTE&CIE, 2009)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3689
_exptl_crystal_description       block
_exptl_crystal_F_000             1249.8930
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.8419
_refine_diff_density_min         -0.5259
_refine_diff_density_rms         0.0681
_refine_ls_d_res_high            0.7829
_refine_ls_d_res_low             7.6282
_refine_ls_goodness_of_fit_ref   0.9932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    112
_refine_ls_number_parameters     692
_refine_ls_number_reflns         12473
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9931
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.0330
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                10351
_reflns_number_total             12473
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b02902_si_002.cif
_cod_data_source_block           3442
_cod_database_code               4132317
_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
 C16, Mo
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 B(H), B'(H')
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C2'(H2'), C7'(H7'), C12'(H12'), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C21'(H21'), C22'(H22'), C23'(H23'),
 C24'(H24'), C25'(H25'), C26'(H26')
3.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), C18(H18a,H18b,H18c), C19(H19a,H19b,
 H19c), C20(H20a,H20b,H20c), C4'(H4'a,H4'b,H4'c), C5'(H5'a,H5'b,H5'c), C9'(H9'a,
 H9'b,H9'c), C10'(H10d,H10e,H10f), C14'(H14d,H14e,H14f), C15'(H15d,H15e,H15f),
 C18'(H18d,H18e,H18f), C19'(H19d,H19e,H19f), C20'(H20d,H20e,H20f)
;
_shelx_res_checksum              2538
_shelx_hkl_checksum              92617
_olex2_submission_special_instructions 'No special instructions were received'