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_7230666
_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_formula_moiety         'C19 H25 N O4'
_chemical_formula_sum            'C19 H25 N O4'
_chemical_formula_weight         331.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1ndsg9
_audit_creation_date             2017-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-08 deposited with the CCDC.
2018-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 106.432(8)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   20.1905(16)
_cell_length_b                   6.6712(4)
_cell_length_c                   12.9057(9)
_cell_measurement_reflns_used    1977
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9610
_cell_measurement_theta_min      3.1570
_cell_volume                     1667.3(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    2.00   38.00   1.0000    3.8950
omega____ theta____ kappa____ phi______ frames
    -       17.1042   38.0000  -60.0000 36

  2 omega   10.00   82.00   1.0000    3.8950
omega____ theta____ kappa____ phi______ frames
    -       17.1042   77.0000    0.0000 72

  3 omega    2.00   84.00   1.0000    3.8950
omega____ theta____ kappa____ phi______ frames
    -       17.1042   38.0000  150.0000 82

  4 omega  -17.00   10.00   1.0000    3.8950
omega____ theta____ kappa____ phi______ frames
    -      -16.2449  -99.0000 -150.0000 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0348325000
_diffrn_orient_matrix_UB_12      -0.0304471000
_diffrn_orient_matrix_UB_13      0.0218633000
_diffrn_orient_matrix_UB_21      0.0060207000
_diffrn_orient_matrix_UB_22      0.0157833000
_diffrn_orient_matrix_UB_23      -0.0509232000
_diffrn_orient_matrix_UB_31      0.0095950000
_diffrn_orient_matrix_UB_32      0.1006418000
_diffrn_orient_matrix_UB_33      0.0145941000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7390
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.111
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61761
_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_density_diffrn    1.320
_exptl_crystal_F_000             712.0
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+3.3400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2420
_refine_ls_wR_factor_ref         0.2640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2646
_reflns_number_total             3809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00481a2.cif
_cod_data_source_block           zdf-56-1
_cod_depositor_comments
'Adding full bibliography for 7230663--7230673.cif.'
_cod_database_code               7230666
_shelxl_version_number           2013-4
_cell_oxdiff_angle_alpha         89.993(5)
_cell_oxdiff_angle_beta          106.466(8)
_cell_oxdiff_angle_gamma         90.003(7)
_cell_oxdiff_length_a            20.193(2)
_cell_oxdiff_length_b            6.6711(4)
_cell_oxdiff_length_c            12.9064(9)
_cell_oxdiff_measurement_reflns_used 1977
_cell_oxdiff_volume              1667.3(2)
_reflns_odcompleteness_completeness 99.95
_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:
 C5(H5), C8(H8), C14(H14), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B), C17(H17A,H17B),
 C19(H19A,H19B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C20(H20), C22(H22)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_olex2_date_sample_data_collection 2017-01-10
_olex2_submission_special_instructions 'No special instructions were received'