Crystal structure of (3S,1'S)-2,2-dimethyl-3-[1,2-cyclohexylidenedioxyethyl]- tetrahydro-1,2-oxazolium tetrafluoroborate, (C~13~H~24~NO~3~)[BF~4~]
W. Frey; M. Henneböhle; V. Jäger; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 149–150; doi:

data_8101672
_publ_section_title
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Crystal structure of (3S,1'S)-2,2-dimethyl-3-[1,2-cyclohexylidenedioxyethyl]-
tetrahydro-1,2-oxazolium tetrafluoroborate, (C~13~H~24~NO~3~)[BF~4~]
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              149
_journal_page_last               150
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C13 H24 B F4 N O3'
_chemical_formula_weight         329.14
_chemical_melting_point          443.5(5)
_chemical_name_systematic
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(3S,1'S)-2,2-dimethyl-3-[1,2-cyclohexylidenedioxyethyl]-tetrahydro-1,2-oxazolium
tetrafluoroborate
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.3197(18)
_cell_length_b                   10.6761(8)
_cell_length_c                   33.786(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      19
_cell_volume                     3361.6(7)
_computing_cell_refinement       'Bruker XScans V. 2.31'
_computing_data_collection       'Bruker XScans V. 2.31'
_computing_data_reduction        'Bruker XScans V. 2.31'
_computing_molecular_graphics    SHELXTL-XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1613
_diffrn_reflns_theta_full        54.97
_diffrn_reflns_theta_max         54.97
_diffrn_reflns_theta_min         2.62
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          1.2
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.9(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.386
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.386
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                1174
_reflns_number_total             1501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1269.cff
_cod_data_source_block           wf706mh
_cod_depositor_comments
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The following automatic conversions were performed:
'_chemical_melting_point' value '443-444 K' changed to '443.5(5)' -
took average value and fixed precision.

Automatic conversion script
Id: cif_fix_values 1543 2011-01-07 15:16:27Z adriana 
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_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               8101672