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_7229556
_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            'C34 H43 F6 N O6 P'
_chemical_formula_weight         706.66
_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                67.011(4)
_cell_angle_beta                 76.108(4)
_cell_angle_gamma                80.955(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6564(11)
_cell_length_b                   13.3543(15)
_cell_length_c                   14.3477(16)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.39
_cell_measurement_theta_min      3.41
_cell_volume                     1649.3(3)
_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 0.973
_diffrn_measured_fraction_theta_max 0.913
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19948
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.962
_diffrn_reflns_theta_min         3.604
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.9410
_exptl_absorpt_correction_T_min  0.8093
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0047(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0620P)^2^+6.7474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5780
_reflns_number_total             6510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01748k2.cif
_cod_data_source_block           1b
_cod_database_code               7229556
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              29814