Reactivity studies of silylene [PhC(NtBu)2](C5Me5)Si - reactions with [M(COD)Cl]2 (M = Rh(i), Ir(i)), S, Se, Te, and BH3.
Kaufmann, Sebastian; Schäfer, Sebastian; Gamer, Michael T.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00483d

data_7042950
_publ_section_title
;
 Reactivity studies of silylene [PhC(NtBu)2](C5Me5)Si - reactions with
 [M(COD)Cl]2 (M = Rh(i), Ir(i)), S, Se, Te, and BH3.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00483d
_journal_year                    2017
_chemical_formula_moiety         'C25 H38 N2 Si Te'
_chemical_formula_sum            'C25 H38 N2 Si Te'
_chemical_formula_weight         522.26
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-03 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.69(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.819(4)
_cell_length_b                   8.7613(18)
_cell_length_c                   29.812(6)
_cell_measurement_reflns_used    17760
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      1.37
_cell_volume                     5174.3(18)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  STOE-STADIVARI
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'single reflection optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            19259
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.067
_diffrn_reflns_theta_min         2.056
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.7870
_exptl_absorpt_correction_T_min  0.4585
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         10010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7590
_reflns_number_total             10010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00483d2.cif
_cod_data_source_block           4new_skp023
_cod_original_cell_volume        5174.4(18)
_cod_database_code               7042950
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C38(H38), C40(H40), C17(H17), C41(H41), C13(H13), C39(H39),
 C16(H16), C15(H15), C14(H14)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C6(H6A,H6B,H6C), C46(H46A,H46B,
 H46C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C50(H50A,H50B,H50C), C48(H48A,
 H48B,H48C), C7(H7A,H7B,H7C), C44(H44A,H44B,H44C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C49(H49A,H49B,H49C), C20(H20A,H20B,H20C), C32(H32A,H32B,
 H32C), C45(H45A,H45B,H45C), C35(H35A,H35B,H35C), C10(H10A,H10B,H10C), C34(H34A,
 H34B,H34C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              42469
_olex2_submission_special_instructions 'No special instructions were received'