Ion-pairing assemblies based on π-extended dipyrrolylquinoxalines
Yamakado, Ryohei; Ishibashi, Haruna; Motoyoshi, Yukari; Yasuda, Nobuhiro; Maeda, Hiromitsu; Chemical Communications  (2018) –; doi:10.1039/C8CC08205G

data_7122688
_publ_section_title
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 Ion-pairing assemblies based on \p-extended dipyrrolylquinoxalines
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08205G
_journal_year                    2018
_chemical_formula_moiety         'C44.46 H55.93 Cl0.93 N5'
_chemical_formula_sum            'C44.46 H55.93 Cl0.93 N5'
_chemical_formula_weight         693.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-05 deposited with the CCDC.
2018-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.064(3)
_cell_length_b                   8.4746(9)
_cell_length_c                   21.388(3)
_cell_measurement_reflns_used    30130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.065
_cell_measurement_theta_min      1.820
_cell_volume                     3999.2(9)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku MercuryCCD2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Si 311'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7007
_diffrn_reflns_av_R_equivalents  0.1661
_diffrn_reflns_av_unetI/netI     0.2189
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30130
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        24.861
_diffrn_reflns_theta_max         27.065
_diffrn_reflns_theta_min         1.820
_diffrn_source                   'synchrotron radiation SPring-8 BL02B1'
_exptl_absorpt_coefficient_mu    0.121
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1494
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1011 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.24(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0426P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.939
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                3329
_reflns_number_total             8664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08205g2.cif
_cod_data_source_block           ydkr_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3999.2(8)
_cod_database_code               7122688
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.995
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              40054