Synthesis and structure of 2,4,6-tricyclobutyl-1,3,5-trioxane
Shorunov, Sergey V.; Bermeshev, Maxim V.; Demchuk, Dmitry V.; Nelyubina, Yulia V.; Acta Crystallographica Section E Crystallographic Communications 75 (2019) 1578–; doi:10.1107/S205698901900896X

data_2021794
_publ_section_title
;
 Synthesis and structure of 2,4,6-tricyclobutyl-1,3,5-trioxane
;
_journal_coeditor_code           KQ2025
_journal_issue                   11
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1578
_journal_paper_doi               10.1107/S205698901900896X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C15 H24 O3'
_chemical_formula_moiety         'C15 H24 O3'
_chemical_formula_sum            'C15 H24 O3'
_chemical_formula_weight         252.34
_chemical_name_systematic
;
2,4,6-Tricyclobutyl-1,3,5-trioxane
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           185
_space_group_name_Hall           'P 6c -2'
_space_group_name_H-M_alt        'P 63 c m'
_symmetry_space_group_name_Hall  'P 6c -2'
_symmetry_space_group_name_H-M   'P 63 c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.9966(12)
_cell_length_b                   9.9966(12)
_cell_length_c                   7.9461(10)
_cell_measurement_reflns_used    7859
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     687.68(15)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>SHELXL2014/6</i> (Sheldrick, 2015b)
;
_computing_publication_material
;
<i>SHELXL2014/6</i> (Sheldrick, 2015b)
;
_computing_structure_refinement
;
<i>SHELXL2014/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII DUO CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.961
_diffrn_reflns_theta_min         2.353
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       prism
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.223
_refine_ls_abs_structure_details 'Refined as an inversion twin'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         671
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0819P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                645
_reflns_number_total             671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            kq2025sup1.cif
_cod_data_source_block           Trioxane
_cod_original_cell_volume        687.68(19)
_cod_database_code               2021794
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              89775
_shelx_res_checksum              95057
_shelxl_version_number           2014/6