Preparation and crystal structures of charge-transfer complexes of acyclic host molecules bearing pyrogallol derivatives with paraquat
Kawahata, Masatoshi; Tominaga, Masahide; Maekawa, Yumi; Yamaguchi, Kentaro; CrystEngComm  (2017) –; doi:10.1039/C7CE01748K

data_7229558
_publ_section_title
;
 Preparation and crystal structures of charge-transfer complexes of
 acyclic host molecules bearing pyrogallol derivatives with paraquat
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01748K
_journal_year                    2017
_chemical_formula_sum            'C45.31 H57.63 F6 N O9.77 P'
_chemical_formula_weight         917.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-09-19 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                83.815(6)
_cell_angle_beta                 84.842(6)
_cell_angle_gamma                76.722(6)
_cell_formula_units_Z            2
_cell_length_a                   9.6535(16)
_cell_length_b                   12.475(2)
_cell_length_c                   18.922(3)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.75
_cell_measurement_theta_min      4.17
_cell_volume                     2199.9(6)
_computing_cell_refinement       'SAINT (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXLE (H\"ubschle et al., 2011)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'BrukerD8 goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28079
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.068
_diffrn_reflns_theta_min         3.655
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.9447
_exptl_absorpt_correction_T_min  0.8622
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADBS Sheldrick 1996'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             967
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         8645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0614P)^2^+1.2763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7306
_reflns_number_total             8645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01748k2.cif
_cod_data_source_block           2b
_cod_database_code               7229558
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              40542