[5,11,17,23-Tetra-<i>tert</i>-butyl-25,27-(3,6-dioxaoctan-1,8-dioxy)-26,28-bis(pyridin-2-ylmethoxy)calix[4]arene]sodium iodide–1,2,4,5-tetrafluoro-3,6-diiodobenzene–methanol (2/3/4)
Cavallo, Gabriella; Metrangolo, Pierangelo; Parisi, Melchiorre F.; Pilati, Tullio; Resnati, Giuseppe; Terraneo, Giancarlo; Acta Crystallographica Section E 69 (2013) m236–m237; doi:10.1107/S1600536813007757

data_2237751
_publ_section_title
;
 [5,11,17,23-Tetra-<i>tert</i>-butyl-25,27-(3,6-dioxaoctan-1,8-dioxy)-26,28-bis(pyridin-2-ylmethoxy)calix[4]arene]sodium
 iodide--1,2,4,5-tetrafluoro-3,6-diiodobenzene--methanol (2/3/4)
;
_journal_coeditor_code           BG2501
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m236
_journal_page_last               m237
_journal_paper_doi               10.1107/S1600536813007757
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '2[Na (C62 H76 N2 O6)]I, 3C6 F4 I2, 4C H4 O'
_chemical_formula_moiety
'2(C62 H76 N2 Na O6 +), 2(I -), 3(C6 F4 I2), 4(C H4 O)'
_chemical_formula_sum            'C146 H168 F12 I8 N4 Na2 O16'
_chemical_formula_weight         3524.02
_chemical_name_systematic
;[5,11,17,23-Tetra-<i>tert</i>-butyl-25,27-(3,6-dioxaoctan-1,8-dioxy)-26,28-bis(pyridin-2-ylmethoxy)calix[4]arene]sodium
iodide--1,2,4,5-tetrafluoro-3,6-diiodobenzene--methanol (2/3/4)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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-2012
_cell_angle_alpha                85.90(2)
_cell_angle_beta                 84.61(2)
_cell_angle_gamma                65.75(2)
_cell_formula_units_Z            1
_cell_length_a                   13.4019(12)
_cell_length_b                   14.2255(12)
_cell_length_c                   21.022(2)
_cell_measurement_reflns_used    33174
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      36.20
_cell_measurement_theta_min      2.46
_cell_volume                     3635.6(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            88833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.428
_diffrn_reflns_theta_min         1.671
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.865460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       prism
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.334
_refine_diff_density_min         -1.519
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         33353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+3.1236P], where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                29534
_reflns_number_total             33353
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2501.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety
'C62 H76 N2 Na O6 +, I -, 1.5(C6 F4 I2), 2(C H4 O)'
_cod_original_formula_iupac      '[Na (C62 H76 N2 O6)] I, 1.5C6 F4 I2, 2C H4 O'
_cod_original_formula_sum        'C73 H84 F6 I4 N2 Na O8'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1762.01
_cod_database_code               2237751
_cod_database_fobs_code          2237751