Chemically-Responsive Complexation of A Diquaternary Salt with Bis(m-phenylene)-32-Crown-10 Derivatives and Host Substituent Effect on Complexation Geometry.
Yan, Xuzhou; Li, Zhengtao; Wei, Peifa; Huang, Feihe; Organic letters 15 (2013) 534–537; doi:10.1021/ol303355z

data_1508881
_publ_section_title
;
 Chemically-Responsive Complexation of A Diquaternary Salt with
 Bis(m-phenylene)-32-Crown-10 Derivatives and Host Substituent Effect on
 Complexation Geometry.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              534
_journal_page_last               537
_journal_paper_doi               10.1021/ol303355z
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C50 H64 O20, C14 H12 N2, 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C68 H82 F12 N4 O20 P2'
_chemical_formula_weight         1565.32
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.548(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9964(10)
_cell_length_b                   13.7356(6)
_cell_length_c                   32.6891(15)
_cell_measurement_reflns_used    4051
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.3877
_cell_measurement_theta_min      2.9568
_cell_volume                     7887.5(7)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            18075
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.9347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     963
_refine_ls_number_reflns         10629
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1773P)^2^+7.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2672
_reflns_number_gt                7454
_reflns_number_total             10629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol303355z_si_002.cif
_cod_data_source_block           120302_yxz_h7g6
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1508881