8,13-Diisopropyl-10,11-dimethyl-bis([1,3]dioxolo[4',5':6,7]naphtho)[1,2-<i>d</i>;2,1-<i>f</i>][1,3]dioxepine
Täufer, Amely; Köckritz, Angela; Quint, Stephan; Spannenberg, Anke; IUCrData 4 (2019) x191018–; doi:10.1107/S2414314619010186

data_1552135
_publ_section_title
;
 8,13-Diisopropyl-10,11-dimethyl-bis([1,3]dioxolo[4',5':6,7]naphtho)[1,2-<i>d</i>;2,1-<i>f</i>][1,3]dioxepine
;
_journal_coeditor_code           HB4307
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x191018
_journal_paper_doi               10.1107/S2414314619010186
_journal_volume                  4
_journal_year                    2019
_chemical_formula_iupac          'C31 H30 O6'
_chemical_formula_moiety         'C31 H30 O6'
_chemical_formula_sum            'C31 H30 O6'
_chemical_formula_weight         498.55
_chemical_name_systematic
8,13-Diisopropyl-10,11-dimethyl-bis([1,3]dioxolo[4',5':6,7]naphtho)[1,2-<i>d</i>;2,1-<i>f</i>][1,3]dioxepine
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                68.0282(16)
_cell_angle_beta                 81.7012(16)
_cell_angle_gamma                86.4672(16)
_cell_formula_units_Z            2
_cell_length_a                   9.7053(6)
_cell_length_b                   11.0901(7)
_cell_length_c                   12.4156(8)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.82
_cell_volume                     1226.25(13)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43308
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.784
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       'part of a plate'
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0747P)^2^+0.4119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                4941
_reflns_number_total             5923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4307sup1.cif
_cod_data_source_block           I
_cod_database_code               1552135
_cod_database_fobs_code          1552135
_shelx_hkl_checksum              32461
_shelx_res_checksum              86759