Centrohexaindane: six benzene rings mutually fixed in three dimensions - solid-state structure and six-fold nitration.
Kuck, Dietmar; Linke, Jens; Teichmann, Lisa Christin; Barth, Dieter; Tellenbröker, Jörg; Gestmann, Detlef; Neumann, Beate; Stammler, Hans-Georg; Bögge, Hartmut; Physical chemistry chemical physics : PCCP 18 (2016) 11722–11737; doi:10.1039/c5cp07005h

data_7223530
_publ_section_title
;
 Centrohexaindane: six benzene rings mutually fixed in three dimensions -
 solid-state structure and six-fold nitration.
;
_journal_issue                   17
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              11722
_journal_page_last               11737
_journal_paper_doi               10.1039/c5cp07005h
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C41 H24, C6 H15 N'
_chemical_formula_sum            'C47 H39 N'
_chemical_formula_weight         617.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-11 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6323(7)
_cell_length_b                   14.7468(7)
_cell_length_c                   14.4198(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.002
_cell_measurement_theta_min      2.366
_cell_volume                     3324.1(3)
_computing_cell_refinement       'SAINT v6.02A (Bruker)'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'SAINT v6.02A (Bruker)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker AXS SMART'
_diffrn_measurement_method       'omega scans'
_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  0.0206
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18458
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.002
_diffrn_reflns_theta_min         1.921
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
? was used for absorption correction.
R(int) was 0.0416 before and 0.0195 after correction.
The Ratio of minimum to maximum transmission is 0.9314.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0797P)^2^+1.9640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3183
_reflns_number_total             3746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cp07005h2.cif
_cod_data_source_block           felsf
_cod_depositor_comments
'Adding full bibliography for 7223530--7223532.cif.'
_cod_database_code               7223530
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H19A(0.5) H19B(0.5) H20B(0.5) H20C(0.5) C21A(0.5) H21A(0.5)
 H21B(0.5) C21B(0.5) H21C(0.5) H21D(0.5) H22F(0.5) H22D(0.5) H22E(0.5)
 H22B(0.5) H22C(0.5) H22A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21A(H21A,H21B), C21B(H21C,H21D)
3.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C), C22(H22F,H22D,H22E), C22(H22B,H22C,H22A)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18)
;
_shelx_res_checksum              4618
_shelx_hkl_checksum              40523
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'