Conformational richness and multiple <i>Z</i>' in salt co-crystal of <i>N</i>-methylpiperidine betaine with <i>N</i>-methylpiperidine betaine hexafluorosilicate
Thaimattam, Ram; Szafran, Miroslaw; Dega-Szafran, Zofia; Jaskolski, Mariusz; Acta Crystallographica Section B 64 (2008) 483–490; doi:10.1107/S0108768108011476

data_2104172
_publ_contact_author
;
      Mariusz Jaskolski
      Department of Crystallography
      Faculty of Chemistry
      A.Mickiewicz University
      Grunwaldzka 6
      60-780 Poznan, Poland
;
_publ_section_title
;
 Conformational richness and multiple <i>Z</i>' in salt co-crystal of
 <i>N</i>-methylpiperidine betaine with <i>N</i>-methylpiperidine
 betaine hexafluorosilicate
;
_journal_coeditor_code           RY5019
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              483
_journal_page_last               490
_journal_paper_doi               10.1107/S0108768108011476
_journal_volume                  64
_journal_year                    2008
_chemical_formula_moiety
'(C8 H15 N1 O2), (C8 H16 N1 O2), 0.5(Si1 F6), (H2 O1)'
_chemical_formula_sum            'C16 H33 F3 N2 O5 Si0.5'
_chemical_formula_weight         404.49
_chemical_melting_point          484.0(10)
_chemical_name_common
;
 N-methylpiperidine betaine hemihexafluorosilicate hydrate
;
_chemical_name_systematic
;
 N-carboxymethyl-N-methylpiperidinium hemihexafluorosilicate hydrate
;
_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                83.87(3)
_cell_angle_beta                 84.81(3)
_cell_angle_gamma                63.86(3)
_cell_formula_units_Z            6
_cell_length_a                   11.554(2)
_cell_length_b                   12.621(3)
_cell_length_c                   22.763(5)
_cell_measurement_reflns_used    27619
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     2959.3(13)
_computing_cell_refinement       'KUMA CCD'
_computing_data_collection       'KUMA CCD'
_computing_data_reduction        'KUMA CrysAlis'
_computing_molecular_graphics    'SHELXTL & PyMOL v0.99'
_computing_publication_material  SHELX-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'KM4 CCD'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27619
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1302.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13415
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                8890
_reflns_number_total             13415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ry5019.cif
_cod_data_source_block           PBETSIF6-II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '
483-485 K' was changed to
'484.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '
483-485 K' was changed to
'484.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2959.2(10)
_cod_database_code               2104172
_cod_database_fobs_code          2104172