Benzo- and Naphthopentalenes: Syntheses, Structures, and Properties.
Kato, Shin-Ichiro; Kuwako, Satoshi; Takahashi, Nobutaka; Kijima, Tomokazu; Nakamura, Yosuke; The Journal of organic chemistry 81 (2016) 7700–7710; doi:10.1021/acs.joc.6b01409

data_4037069
_publ_section_title
;
 Benzo- and Naphthopentalenes: Syntheses, Structures, and Properties.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              7700
_journal_page_last               7710
_journal_paper_doi               10.1021/acs.joc.6b01409
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C60 H58'
_chemical_formula_weight         779.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4783(9)
_cell_length_b                   27.727(2)
_cell_length_c                   35.544(3)
_cell_measurement_reflns_used    6215
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      30.7
_cell_volume                     9341.1(14)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            50555
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.391
_diffrn_reflns_theta_min         6.180
_exptl_absorpt_coefficient_mu    0.465
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0652P)^2^+2.9370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7340
_reflns_number_total             8501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01409_si_005.cif
_cod_data_source_block           sk020
_cod_database_code               4037069
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2014/6
_shelx_res_checksum              10328
_shelx_hkl_checksum              74854