3,3,6,6,9,9-Hexaethyl-1,2,4,5,7,8-hexaoxacyclononane at 296 K
Cerna, Jorge; Bernès, Sylvain; Cañizo, Adriana; Eyler, Nora; Acta Crystallographica Section C 65 (2009) o562–o564; doi:10.1107/S0108270109039833

data_2017418
_publ_section_title
;
 3,3,6,6,9,9-Hexaethyl-1,2,4,5,7,8-hexaoxacyclononane at 296 K
;
_journal_coeditor_code           UK3010
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o562
_journal_page_last               o564
_journal_paper_doi               10.1107/S0108270109039833
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C15 H30 O6'
_chemical_formula_moiety         'C15 H30 O6'
_chemical_formula_sum            'C15 H30 O6'
_chemical_formula_weight         306.39
_chemical_melting_point_gt       332
_chemical_melting_point_lt       333
_chemical_name_common            'Diethyl ketone triperoxide'
_chemical_name_systematic
;
3,3,6,6,9,9-Hexaethyl-1,2,4,5,7,8-hexaoxacyclononane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.796(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.4545(12)
_cell_length_b                   10.859(3)
_cell_length_c                   32.168(5)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      4.66
_cell_volume                     3650.1(12)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Version 2.0; Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17260
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        >50
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.145
_refine_ls_extinction_coef       0.0046(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.5376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                4356
_reflns_number_total             6424
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3010.cif
_cod_data_source_block           I
_cod_original_cell_volume        3650.0(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017418
_cod_database_fobs_code          2017418