What is responsible for conformational diversity in single-crystal tetraoxazaspiroalkanes? X-Ray, DFT, and AIM approaches
Tulyabaev, Arthur R.; Bikmukhametov, Kamil Sh.; Mescheryakova, Ekaterina S.; Makhmudiyarova, Natalia N.; Rakhimov, Rustem Sh.; Khalilov, Leonard M.; CrystEngComm 20 (2018) 3207–; doi:10.1039/C8CE00481A

data_7230663
_publ_section_title
;
 What is responsible for conformational diversity in single-crystal
 tetraoxazaspiroalkanes? X-Ray, DFT, and AIM approaches
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              3207
_journal_paper_doi               10.1039/C8CE00481A
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C15 H20 F N O4'
_chemical_formula_sum            'C15 H20 F N O4'
_chemical_formula_weight         297.32
_chemical_name_systematic
11-(4-fluorophenyl)-8,9,13,14-tetraoxa-11-azaspiro[6.7]tetradecane
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc14mwn9
_audit_creation_date             2015-04-27
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2015-04-27 deposited with the CCDC.
2018-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.329(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.7993(5)
_cell_length_b                   25.037(3)
_cell_length_c                   10.1500(11)
_cell_measurement_reflns_used    421
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.6355
_cell_measurement_theta_min      1.6193
_cell_volume                     1449.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1709
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega    5.00   54.00   1.0000   23.2100
omega____ theta____ kappa____ phi______ frames
    -       24.2348   57.0000  150.0000 49

  2 omega  -46.00   54.00   1.0000   23.2100
omega____ theta____ kappa____ phi______ frames
    -       24.2348  -77.0000 -180.0000 100

  3 omega  -38.00   -2.00   1.0000   23.2100
omega____ theta____ kappa____ phi______ frames
    -       24.2348  -77.0000  -90.0000 36

  4 omega   -7.00   18.00   1.0000   23.2100
omega____ theta____ kappa____ phi______ frames
    -       24.2348   81.0000  146.0000 25

  5 omega   -3.00   86.00   1.0000   23.2100
omega____ theta____ kappa____ phi______ frames
    -       24.2348   77.0000  -60.0000 89

  6 omega    1.00   94.00   1.0000   23.2100
omega____ theta____ kappa____ phi______ frames
    -       24.2348   77.0000   30.0000 93
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1263206000
_diffrn_orient_matrix_UB_12      -0.0188940000
_diffrn_orient_matrix_UB_13      -0.0048961000
_diffrn_orient_matrix_UB_21      0.0201063000
_diffrn_orient_matrix_UB_22      0.0377733000
_diffrn_orient_matrix_UB_23      -0.0476149000
_diffrn_orient_matrix_UB_31      0.0009092000
_diffrn_orient_matrix_UB_32      0.0570567000
_diffrn_orient_matrix_UB_33      0.0300526000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5439
_diffrn_reflns_theta_full        30.93
_diffrn_reflns_theta_max         30.93
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'XCalibur Eos'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             776
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.7(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         2662
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                2247
_reflns_number_total             2662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00481a2.cif
_cod_data_source_block           rr-250-9
_cod_depositor_comments
'Adding full bibliography for 7230663--7230673.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7230663