Stable and twisted 5,6:12,13-dinaphthozethrene from angular π-extension.
Hu, Jinlian; Xiang, Qin; Xu, Jun; Xu, Zhanqiang; Chen, Guang; Sun, Zhe; Chemical communications (Cambridge, England) 57 (2021) 9712–9715; doi:10.1039/d1cc04113d

data_7128925
_publ_section_title
;
 Stable and twisted 5,6:12,13-dinaphthozethrene from angular \p-extension.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9712
_journal_page_last               9715
_journal_paper_doi               10.1039/d1cc04113d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C58 H42, C7 H8'
_chemical_formula_sum            'C65 H50'
_chemical_formula_weight         831.05
_chemical_properties_physical
Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-08
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.05.01 svn.r6f5a8f70 for OlexSys, GUI svn.r6320)
;
_audit_update_record
;
2021-06-18 deposited with the CCDC.	2021-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.31790(10)
_cell_length_b                   11.15600(10)
_cell_length_c                   27.3475(2)
_cell_measurement_reflns_used    97370
_cell_measurement_temperature    160
_cell_measurement_theta_max      74.2910
_cell_measurement_theta_min      1.6480
_cell_volume                     5771.07(8)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      160
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'ROD,Synergy Custom system Hypix'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            201132
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.874
_diffrn_reflns_theta_min         2.572
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56943
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.956
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00098(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         11631
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+1.2279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10429
_reflns_number_total             11631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04113d2.cif
_cod_data_source_block           s1-0408
_cod_depositor_comments          'Adding full bibliography for 7128925.cif.'
_cod_database_code               7128925
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.941
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C45(H45), C52(H52),
 C54(H54), C01H(H01H), C01K(H01K), C01N(H01N), C01O(H01O), C017(H017)
3.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C01P(H01A,H01B,H01C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96225
_shelx_hkl_checksum              69771
_shelx_fab_checksum              62791
_olex2_submission_special_instructions 'No special instructions were received'