Monoreduced 1,2-dihydrocorannulene <i>versus</i> the parent corannulene
Spisak, Sarah N.; Hoover, Gabrielle C.; Wei, Zheng; Zabula, Alexander V.; Filatov, Alexander S.; Petrukhina, Marina A.; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615013145

data_2020058
_publ_section_title
;
 Monoreduced 1,2-dihydrocorannulene <i>versus</i> the parent corannulene
;
_journal_coeditor_code           FA3372
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615013145
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[K (C6 H14 O3)3] (C20 H12)'
_chemical_formula_moiety         'C18 H42 K O9 +, C20 H12 -'
_chemical_formula_sum            'C38 H54 K O9'
_chemical_formula_weight         693.91
_chemical_name_common
;Tris(diglyme-\k^3^<i>O</i>,<i>O</i>',<i>O</i>'')potassium
1,2-dihydrocorannulenide
;
_chemical_name_systematic
;Tris[1-methoxy-2-(2-methoxyethoxy)ethane-\k^3^<i>O</i>,<i>O</i>',<i>O</i>'']potassium
hexacyclo[11.5.2.0^4,17^.0^7,16^.0^10,15^.0^14,18^]icosa-1,3,5,7(16),8,10(15),11,13,17-nonaenide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.7310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5274(8)
_cell_length_b                   15.4463(13)
_cell_length_c                   12.7366(11)
_cell_measurement_reflns_used    5340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.67
_cell_measurement_theta_min      2.16
_cell_volume                     1852.6(3)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2003)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Bruker, 2003)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16228
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         1.618
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.837060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2003)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.342
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2042 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8319
_refine_ls_number_restraints     326
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0870P)^2^+0.4677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                5599
_reflns_number_total             8319
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3372sup1.cf
_cod_data_source_block           I
_cod_database_code               2020058
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              23312
_shelx_res_checksum              738
_shelxl_version_number           2014/6
_cod_database_fobs_code 2020058