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_2014691
_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 H38 N2 O4'
_chemical_formula_moiety         'C26 H38 N2 O4'
_chemical_formula_sum            'C26 H38 N2 O4'
_chemical_formula_weight         442.58
_chemical_melting_point          80.5(5)
_chemical_name_common
;
N,N'-Dibenzyl-4,13-diaza-18-crown-6
;
_chemical_name_systematic
;
7,16-Dibenzyl-1,4,10,13-tetraoxo-7,16-diazacyclooctadecane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.993(3)
_cell_length_b                   22.455(5)
_cell_length_c                   13.391(3)
_cell_measurement_reflns_used    15860
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1
_cell_volume                     4968.9(19)
_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-3 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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25950
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0764
_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^)+(0.0426P)^2^+2.1759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                5565
_reflns_number_total             8591
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1362.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '80--81' was changed to '80.5(5)' -
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 '80--81' was changed to '80.5(5)' -
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_cell_volume        4968.9(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2014691
_cod_database_fobs_code          2014691