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_7042953
_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         'C33 H50 Cl Ir N2 Si'
_chemical_formula_sum            'C33 H50 Cl Ir N2 Si'
_chemical_formula_weight         730.49
_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
_audit_creation_date             2017-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-08 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.076(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9611(5)
_cell_length_b                   12.5782(3)
_cell_length_c                   21.1334(8)
_cell_measurement_reflns_used    13631
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      1.90
_cell_volume                     3171.46(19)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110
_diffrn_detector                 'Dectris Pilatus 100k'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17593
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.872
_diffrn_reflns_theta_min         1.885
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    4.356
_exptl_absorpt_correction_T_max  0.3625
_exptl_absorpt_correction_T_min  0.2663
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.223
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0237P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5539
_reflns_number_total             7813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00483d2.cif
_cod_data_source_block           5-SebSK07-2
_cod_database_code               7042953
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C21A(0.6) H21A(0.6) H21B(0.6) H21C(0.6) C19A(0.6) H19A(0.6)
 H19B(0.6) H19C(0.6) C20A(0.6) H20A(0.6) H20B(0.6) H20C(0.6) C19B(0.4)
 H19D(0.4) H19E(0.4) H19F(0.4) C20B(0.4) H20D(0.4) H20E(0.4) H20F(0.4)
 C21B(0.4) H21D(0.4) H21E(0.4) H21F(0.4)
3.a Ternary CH refined with riding coordinates:
 C30(H30), C31(H31), C27(H27), C26(H26)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C36(H36A,H36B), C28(H28A,H28B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C16(H16), C15(H15), C14(H14)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C),
 C24(H24A,H24B,H24C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C),
 C21A(H21A,H21B,H21C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C19B(H19D,
 H19E,H19F), C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F)
;
_shelx_res_checksum              92641
_olex2_submission_special_instructions 'No special instructions were received'