Synthesis, Characterization, and Solid-State Structure of [8]Cycloparaphenylenes with Inherent Chirality.
Della Sala, Paolo; Talotta, Carmen; De Rosa, Margherita; Soriente, Annunziata; Geremia, Silvano; Hickey, Neal; Neri, Placido; Gaeta, Carmine; The Journal of organic chemistry 84 (2019) 9489–9496; doi:10.1021/acs.joc.9b01026

data_4034394
_publ_section_title
;
 Synthesis, Characterization, and Solid-State Structure of
 [8]Cycloparaphenylenes with Inherent Chirality.
;
_journal_issue                   15
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9489
_journal_page_last               9496
_journal_paper_doi               10.1021/acs.joc.9b01026
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C49  H34, 2(C H2 Cl2)'
_chemical_formula_sum            'C51 H38 Cl4'
_chemical_formula_weight         792.61
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2019-02-01T13:34:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.527(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.485(3)
_cell_length_b                   9.779(4)
_cell_length_c                   26.384(4)
_cell_measurement_reflns_used    39062
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      0.77
_cell_measurement_wavelength     0.7
_cell_volume                     3969.4(19)
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'Area Detector'
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            62141
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         28.318
_diffrn_reflns_theta_min         0.765
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.064(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     558
_refine_ls_number_reflns         62141
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1455P)^2^+3.8924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2725
_reflns_Friedel_coverage         0
_reflns_number_gt                47107
_reflns_number_total             62141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01026_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3969.4(18)
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4034394