5,7,8,10,11,13,14,16-Octahydro-6,15-(ethanoxyethanoxyethano)-1,4:17,20-dietheno[9,12,6,15]benzodioxadiazacyclodocosine
Barnett, Heath A.; Fronczek, Frank R.; Watkins, Steven F.; Acta Crystallographica Section E 68 (2012) o3239–; doi:10.1107/S1600536812044017

data_2236142
_publ_section_title
;
 5,7,8,10,11,13,14,16-Octahydro-6,15-(ethanoxyethanoxyethano)-1,4:17,20-dietheno[9,12,6,15]benzodioxadiazacyclodocosine
;
_journal_coeditor_code           BV2212
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3239
_journal_paper_doi               10.1107/S1600536812044017
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C32 H40 N2 O4'
_chemical_formula_moiety         'C32 H40 N2 O4'
_chemical_formula_sum            'C32 H40 N2 O4'
_chemical_formula_weight         516.66
_chemical_name_common
;
5,7,8,10,11,13,14,16-Octahydro-6,15-(ethanoxyethanoxyethano)-1,4:17,20-\
dietheno[9,12,6,15]benzodioxadiazacyclodocosine
;
_chemical_name_systematic
;
21,24,29,32-Tetraoxa-1,18-
diazapentacyclo[16.8.8.2^3,6^.2^13,16^.0^7,12^]octatriaconta-
3,5,7(12),8,10,13,15,35,37-nonaene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                88.178(2)
_cell_angle_beta                 82.616(2)
_cell_angle_gamma                78.072(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6757(3)
_cell_length_b                   12.1582(4)
_cell_length_c                   12.5129(5)
_cell_measurement_pressure       101.3
_cell_measurement_reflns_used    10814
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      33.142
_cell_measurement_theta_min      2.546
_cell_volume                     1428.26(9)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10763
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         33.1
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.9829
_exptl_absorpt_correction_T_min  0.9745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.224
_refine_ls_extinction_coef       0.0078(12)
_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   0.806
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     351
_refine_ls_number_reflns         10763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                5346
_reflns_number_total             10763
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bv2212.cif
_cod_data_source_block           I
_cod_database_code               2236142
_cod_database_fobs_code          2236142