Solution and Gas-Phase Investigations of Trimethylsilylpropyl-Substituted Pyridinium Ions. Manifestation of the Silicon δ Effect
Karnezis, Asimo; O’Hair, Richard A. J.; White, Jonathan M.; Organometallics 30 (2011) 5665–; doi:10.1021/om200510a

data_4065020
_publ_section_title
;
 Solution and Gas-Phase Investigations of Trimethylsilylpropyl-Substituted
 Pyridinium Ions. Manifestation of the Silicon \d Effect
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5665
_journal_paper_doi               10.1021/om200510a
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C17 H22 N4 O7 Si'
_chemical_formula_weight         422.48
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.444(9)
_cell_angle_beta                 98.291(11)
_cell_angle_gamma                94.511(10)
_cell_formula_units_Z            2
_cell_length_a                   6.7542(10)
_cell_length_b                   11.2277(12)
_cell_length_c                   13.9266(16)
_cell_measurement_reflns_used    1534
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      73.8809
_cell_measurement_theta_min      3.2048
_cell_volume                     1041.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6822
_diffrn_reflns_theta_full        67.48
_diffrn_reflns_theta_max         67.48
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.2246
_exptl_crystal_size_mid          0.1213
_exptl_crystal_size_min          0.0653
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+0.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2148
_reflns_number_gt                2699
_reflns_number_total             3757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200510a_si_002.cif
_cod_data_source_block           jmwak100
_cod_database_code               4065020