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_4132315
_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 Mo N6 O2 P, C7 H8'
_chemical_formula_sum            'C27 H39 B Mo N6 O2 P'
_chemical_formula_weight         617.36
_chemical_name_systematic        PG-180
_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   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                109.370(2)
_cell_angle_beta                 93.449(3)
_cell_angle_gamma                98.756(3)
_cell_formula_units_Z            4
_cell_length_a                   13.5487(4)
_cell_length_b                   14.7499(5)
_cell_length_c                   16.1417(5)
_cell_measurement_reflns_used    17864
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.94
_cell_volume                     2986.48(17)
_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 0.988
_diffrn_measured_fraction_theta_max 0.985
_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  0.0569
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28355
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.937
_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    0.527
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_correction_T_min  0.9111
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       rod
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.824
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         14213
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0583
_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^)+(0.1083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10499
_reflns_number_total             14213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02902_si_002.cif
_cod_data_source_block           2280
_cod_database_code               4132315
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C21' \\sim C22' \\sim C23' \\sim C24' \\sim C25' \\sim C26' \\sim C27': within
2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C21') \\sim Ueq, Uanis(C22') \\sim Ueq, Uanis(C23') \\sim Ueq,
Uanis(C24') \\sim Ueq, Uanis(C25') \\sim Ueq, Uanis(C26') \\sim Ueq,
Uanis(C27') \\sim Ueq, Uanis(C16') \\sim Ueq, Uanis(C17') \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C2'(H2'), C7'(H7'), C12'(H12'), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C22'(H22'), C23'(H23'), C24'(H24'), C25'(H25'),
 C26'(H26')
3.b 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), 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),
 C16'(H16D,H16E,H16F), C17'(H17D,H17E,H17F), C18'(H18D,H18E,H18F), C27(H27A,
 H27B,H27C), C27'(H27D,H27E,H27F)
;
_shelx_res_checksum              91619
_shelx_hkl_checksum              61804
_olex2_submission_special_instructions 'No special instructions were received'