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_1508880
_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
'C52 H60 Fe2 O14, C14 H12 N2, 2(F6 P), C3 H6 O '
_chemical_formula_sum            'C69 H78 F12 Fe2 N2 O15 P2'
_chemical_formula_weight         1576.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8315(6)
_cell_length_b                   10.7382(3)
_cell_length_c                   29.5987(7)
_cell_measurement_reflns_used    11176
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.4444
_cell_measurement_theta_min      2.9490
_cell_volume                     6938.9(3)
_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      170(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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34051
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_correction_T_min  0.8401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         11730
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+3.4331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                10369
_reflns_number_total             11730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol303355z_si_002.cif
_cod_data_source_block           120920_h12g1
_cod_original_cell_volume        6938.8(3)
_cod_database_code               1508880