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_7230670
_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 ad
_chemical_formula_moiety         'C18 H26 Cl N O4'
_chemical_formula_sum            'C18 H26 Cl N O4'
_chemical_formula_weight         355.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.111(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5582(8)
_cell_length_b                   6.0006(3)
_cell_length_c                   27.226(2)
_cell_measurement_reflns_used    2244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5280
_cell_measurement_theta_min      1.8730
_cell_volume                     1852.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1709
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -23.00    3.00   1.0000   25.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.2449  -99.0000 -180.0000 26

  2 omega  -35.00   27.00   1.0000   25.3700
omega____ theta____ kappa____ phi______ frames
    -       16.9480  -57.0000  -90.0000 62

  3 omega  -42.00   84.00   1.0000   25.3700
omega____ theta____ kappa____ phi______ frames
    -       16.9480    0.0000  120.0000 126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0373112000
_diffrn_orient_matrix_UB_12      0.0742294000
_diffrn_orient_matrix_UB_13      0.0160465000
_diffrn_orient_matrix_UB_21      -0.0413821000
_diffrn_orient_matrix_UB_22      0.0038864000
_diffrn_orient_matrix_UB_23      0.0161533000
_diffrn_orient_matrix_UB_31      0.0284208000
_diffrn_orient_matrix_UB_32      -0.0919792000
_diffrn_orient_matrix_UB_33      0.0136072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            9047
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.251
_diffrn_reflns_theta_min         1.796
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       needle
_exptl_crystal_F_000             760.0
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1257 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6850
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0746P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4464
_reflns_number_total             6850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00481a2.cif
_cod_data_source_block           kls-14-4
_cod_depositor_comments
'Adding full bibliography for 7230663--7230673.cif.'
_cod_database_code               7230670
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13'(H13'), C14'(H14'), C10'(H10')
2.b Secondary CH2 refined with riding coordinates:
 C9'(H9'A,H9'B), C11'(H11C,H11D), C5'(H5'A,H5'B), C3'(H3'A,H3'B), C12'(H12C,
 H12D)
2.c Aromatic/amide H refined with riding coordinates:
 C19'(H19'), C20'(H20'), C22'(H22'), C23'(H23')
2.d Idealised Me refined as rotating group:
 C17'(H17D,H17E,H17F), C16(H16A,H16B,H16C), C16'(H16D,H16E,H16F), C15'(H15D,
 H15E,H15F), C15(H15A,H15B,H15C)
;
_olex2_date_sample_data_collection 2017-11-14
_olex2_submission_special_instructions 'No special instructions were received'