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_4037068
_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            'C60.5 H59 Cl'
_chemical_formula_weight         821.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                86.666(11)
_cell_angle_beta                 72.882(7)
_cell_angle_gamma                82.504(10)
_cell_formula_units_Z            4
_cell_length_a                   16.676(2)
_cell_length_b                   16.766(2)
_cell_length_c                   18.310(2)
_cell_measurement_reflns_used    16997
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5010
_cell_measurement_theta_min      3.0038
_cell_volume                     4849.6(10)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Varimax Saturn70'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78517
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.004
_exptl_absorpt_coefficient_mu    0.116
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         17030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0956
_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^)+(0.0553P)^2^+4.6482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14693
_reflns_number_total             17030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01409_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        4849.7(12)
_cod_original_formula_sum        'C60.50 H59 Cl'
_cod_database_code               4037068
_shelx_estimated_absorpt_t_min   0.985
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2014/6
_shelx_res_checksum              17381
_shelx_hkl_checksum              9078