Tris(dimethylamino)silylium ion: structure and reactivity of a dimeric silaguanidinium
Kramer, Nina; Wadepohl, Hubert; Greb, Lutz; Chemical Communications  (2019) –; doi:10.1039/C9CC03625C

data_7123643
_publ_section_title
;
 Tris(dimethylamino)silylium ion: structure and reactivity of a dimeric
 silaguanidinium
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03625C
_journal_year                    2019
_chemical_formula_moiety         'C16 H28 Fe N3 Si, B C24 F20'
_chemical_formula_sum            'C40 H28 B F20 Fe N3 Si'
_chemical_formula_weight         1025.40
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                nk536
_audit_creation_date             2019-05-08
_audit_creation_method
; 
Olex2 1.2 
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2019-05-09 deposited with the CCDC.    2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.990(2)
_cell_length_b                   18.213(4)
_cell_length_c                   22.061(4)
_cell_measurement_reflns_used    1995
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.0
_cell_volume                     4011.0(14)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius and Bruker AXS, 1997-2009)'
_computing_data_reduction
'DENZO/SCALEPACK (Otwinowski & Minor, 1997), SADABS (Sheldrick and Bruker AXS, 2004)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69147
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              "'fine focus tube' "
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.750
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0415P)^2^+2.0402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6775
_reflns_number_total             9957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03625c2.cif
_cod_data_source_block           nk536
_cod_database_code               7123643
_audit_block_usercomment         nk536
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.689
_shelxl_version_number           2018/3
_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 Idealised Me refined as rotating group with stretchable bonds: 
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B, 
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C) 
;
_shelx_res_checksum              51496