A new phase of 7,16-dibenzyl-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane, and 7,16-dibenzyl-1,4,10,13-tetraoxa-7,16-diazoniacyclooctadecane bis(tetrafluoroborate) monohydrate, both determined at 123K
Basok, Stepan S.; Croitoru Lilia; Fonari, Marina S.; Ganin, Eduard V.; Gelmboldt, Vladimir O.; Lipkowski, Janusz; Simonov, Yurii A.; Acta Crystallographica Section C 61 (2005) o188–o192; doi:10.1107/S010827010500260X

data_2014692
_publ_section_title
;
 A new phase of
 7,16-dibenzyl-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane, and
 7,16-dibenzyl-1,4,10,13-tetraoxa-7,16-diazoniacyclooctadecane
 bis(tetrafluoroborate) monohydrate, both determined at 123K
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o188
_journal_page_last               o192
_journal_paper_doi               10.1107/S010827010500260X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C26 H40 N2 O4 2+, 2B F4 -, H2 O'
_chemical_formula_moiety         'C26 H40 N2 O4, 2B F4, H2 O'
_chemical_formula_sum            'C26 H40 B2 F8 N2 O4.2'
_chemical_formula_weight         621.48
_chemical_melting_point          169.0(10)
_chemical_name_common
;
 N,N'-dibenzyl-1,4,10,13-tetraoxa-7,16-diazoniacyclooctadecane
 bis tetrafluoroborate monohydrate
;
_chemical_name_systematic
;
 N,N'-dibenzyl-1,4,10,13-tetraoxa-7,16-diazoniacyclooctadecane
 bis tetrafluoroborate monohydrate
;
_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                69.342(4)
_cell_angle_beta                 72.226(4)
_cell_angle_gamma                81.480(4)
_cell_formula_units_Z            1
_cell_length_a                   7.9290(6)
_cell_length_b                   9.3870(6)
_cell_length_c                   11.6070(7)
_cell_measurement_reflns_used    3035
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1
_cell_volume                     768.98(9)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'ORTEP for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
' Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       '\f and \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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4974
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             326
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.1724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                2159
_reflns_number_total             2660
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1362.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '168--170' was changed to '169.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '168--170' was changed to '169.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C26 H40 B2 F8 N2 O4.20'
_cod_database_code               2014692
_cod_database_fobs_code          2014692