Invariom-model refinement and Hirshfeld surface analysis of well-ordered solvent-free dibenzo-21-crown-7
Wiedemann, Dennis; Kohl, Julia; Acta Crystallographica Section C Structural Chemistry 73 (2017) –; doi:10.1107/S2053229617011160

data_2020840
_publ_section_title
;
 Invariom-model refinement and Hirshfeld surface analysis of well-ordered
 solvent-free dibenzo-21-crown-7
;
_journal_coeditor_code           SK3663
_journal_issue                   9
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229617011160
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C22 H28 O7'
_chemical_formula_moiety         'C22 H28 O7'
_chemical_formula_sum            'C22 H28 O7'
_chemical_formula_weight         404.44
_chemical_melting_point          388
_chemical_name_common            dibenzo-21-crown-7
_chemical_name_systematic
;
Dibenzo[<i>b</i>,<i>k</i>][1,4,7,10,13,16,19]heptaoxacyclohenicosa-2,11-diene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 94.1240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.98010(10)
_cell_length_b                   17.4771(2)
_cell_length_c                   23.1000(2)
_cell_measurement_reflns_used    7438
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.509
_cell_measurement_theta_min      2.514
_cell_volume                     2005.37(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
WinXD (Volkov <i>et al.</i>,  2016)
;
_computing_structure_refinement
;
XD2016 (Volkov <i>et al.</i>,  2016)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.5435
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (single source)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13236
_diffrn_reflns_theta_full        67.5
_diffrn_reflns_theta_max         73.657
_diffrn_reflns_theta_min         3.174
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.34
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.738
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9807
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3664
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.1P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                3559
_reflns_number_total             3925
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3663sup1.cif
_cod_data_source_block           Invariom
_cod_database_code               2020840
_cod_database_fobs_code          2020840