Crystallization of cesium complex containing bis(2-propyloxy)calix[4]crown-6 and bis[(trifluoromethyl)sulfonyl]imide
Taoxiang Sun; Zheming Wang; Xinghai Shen; Inorganica Chimica Acta 390 (2012) 8–11; doi:10.1016/j.ica.2012.04.005

data_1512426
_publ_section_title
;
 Crystallization of cesium complex containing
 bis(2-propyloxy)calix[4]crown-6 and bis[(trifluoromethyl)sulfonyl]imide
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              8
_journal_page_last               11
_journal_paper_doi               10.1016/j.ica.2012.04.005
_journal_volume                  390
_journal_year                    2012
_chemical_formula_sum            'C46 H54 Cs F6 N O12 S2'
_chemical_formula_weight         1123.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.2114(8)
_cell_angle_beta                 87.9841(7)
_cell_angle_gamma                89.4630(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6429(2)
_cell_length_b                   13.5876(3)
_cell_length_c                   17.5651(4)
_cell_measurement_reflns_used    19201
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.395
_cell_volume                     2532.93(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33523
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0015(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         8940
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                5142
_reflns_number_total             8940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012_390-8-11.cif
_cod_data_source_block           10aug27b
_cod_database_code               1512426