Capturing the Fused-Pentagon C74 by Stepwise Chlorination.
Gao, Cong-Li; Abella, Laura; Tan, Yuan-Zhi; Wu, Xin-Zhou; Rodríguez-Fortea, Antonio; Poblet, Josep M.; Xie, Su-Yuan; Huang, Rong-Bin; Zheng, Lan-Sun; Inorganic chemistry 55 (2016) 6861–6865; doi:10.1021/acs.inorgchem.5b02824

data_4347168
_publ_section_title
;
 Capturing the Fused-Pentagon C74 by Stepwise Chlorination.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6861
_journal_page_last               6865
_journal_paper_doi               10.1021/acs.inorgchem.5b02824
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C81 H8 Cl10'
_chemical_formula_weight         1335.37
_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
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 95.177(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2877(7)
_cell_length_b                   19.4374(10)
_cell_length_c                   23.9460(11)
_cell_measurement_reflns_used    7834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.3592
_cell_measurement_theta_min      0.9825
_cell_volume                     4768.9(5)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16153
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         64.360
_diffrn_reflns_theta_min         3.707
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.845
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91774
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.717
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         7834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1150P)^2^+17.6730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6689
_reflns_number_total             7834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02824_si_002.cif
_cod_data_source_block           p
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347168
_shelxl_version_number           2014-1
_shelx_res_checksum              26290
_shelx_hkl_checksum              42797