New synthesis of tetraoxaspirododecane-diamines and tetraoxazaspirobicycloalkanes
Makhmudiyarova, Nataliya N.; Shangaraev, Kamil R.; Dzhemileva, Lilya U.; Tyumkina, Tatyana V.; Mescheryakova, Ekaterina S.; D'yakonov, Vladimir A.; Ibragimov, Askhat G.; Dzhemilev, Usein M.; RSC Advances 9 (2019) 29949–; doi:10.1039/C9RA06372B

data_7234166
_publ_section_title
;
 New synthesis of tetraoxaspirododecane-diamines and
 tetraoxazaspirobicycloalkanes
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              29949
_journal_paper_doi               10.1039/C9RA06372B
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C8 H14 O6'
_chemical_formula_sum            'C8 H14 O6'
_chemical_formula_weight         206.19
_chemical_name_systematic        7,8,11-trioxaspiro[5.6]dodecane-9,10-diol
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.5986(6)
_cell_length_b                   9.8591(8)
_cell_length_c                   29.604(2)
_cell_measurement_reflns_used    1039
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1750
_cell_measurement_theta_min      2.7480
_cell_volume                     1925.9(3)
_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
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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    'ShelXD (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  -24.00   23.00   0.5000   25.1550
omega____ theta____ kappa____ phi______ frames
    -      -16.2449  -99.0000 -150.0000 94

  2 omega   46.00   82.00   0.5000   25.1550
omega____ theta____ kappa____ phi______ frames
    -       16.9480   57.0000   60.0000 72

  3 omega    8.00   78.00   0.5000   25.1550
omega____ theta____ kappa____ phi______ frames
    -       16.9480   57.0000  -30.0000 140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0943885000
_diffrn_orient_matrix_UB_12      -0.0227918000
_diffrn_orient_matrix_UB_13      -0.0085252000
_diffrn_orient_matrix_UB_21      -0.0433968000
_diffrn_orient_matrix_UB_22      -0.0073917000
_diffrn_orient_matrix_UB_23      -0.0217850000
_diffrn_orient_matrix_UB_31      0.0272571000
_diffrn_orient_matrix_UB_32      0.0678509000
_diffrn_orient_matrix_UB_33      -0.0052483000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_max 0.739
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            4693
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.051
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'XCalibur E'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15846
_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    1.422
_exptl_crystal_description       prizm
_exptl_crystal_F_000             880.0
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                750
_reflns_number_total             1905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra06372b2.cif
_cod_data_source_block           iir-297-13_twin1_hklf4
_cod_database_code               7234166
_shelxl_version_number           2013-4
_diffrn_oxdiff_twin_integration_method simultaneous
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C005(H005), C008(H008)
2.b Secondary CH2 refined with riding coordinates:
 C010(H01A,H01B), C011(H01C,H01D), C012(H01E,H01F), C013(H01G,H01H), C014(H01I,
 H01J)
2.c Idealised tetrahedral OH refined as rotating group:
 O002(H002), O003(H003)
;