A Schiff base lateral macrobicycle derived from 4,13-diaza-18-crown-6 in its protonated form
Avecilla, Fernando; Esteban, David; Platas-Iglesias, Carlos; Fernández-Martínez, Susana; De Blas, Andres; Rodríguez-Blas, Teresa; Acta Crystallographica Section C 61 (2005) o92–o94; doi:10.1107/S0108270104033657

data_2014645
_publ_section_title
;
 A Schiff base lateral macrobicycle derived from 4,13-diaza-18-crown-6
 in its protonated form
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o92
_journal_page_last               o94
_journal_paper_doi               10.1107/S0108270104033657
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C33 H43 N5 O4 2+ , 2Cl O4 -'
_chemical_formula_moiety         'C33 H43 N5 O4 2+ , 2Cl O4 -'
_chemical_formula_sum            'C33 H43 Cl2 N5 O12'
_chemical_formula_weight         772.62
_chemical_name_systematic
;
28,31,36,39-tetraoxa-9,17,42-pentaaza-1,25-
diazoniapentacyclo[23.8.5.1^11,15^.0^3,8^.0^18,23^]nonatriaconta-
3,5,7,9,11,13,15,16,18,20,22-undecane bis(perchlorate)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.8800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5092(2)
_cell_length_b                   19.1979(2)
_cell_length_c                   20.6024(5)
_cell_measurement_reflns_used    951
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.86
_cell_volume                     3734.02(13)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1997a)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13616
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0.39
_diffrn_standards_interval_count 'set of frames'
_diffrn_standards_number         'first 50 frames'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.9312
_exptl_absorpt_correction_T_min  0.9097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-like
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.588
_refine_ls_extinction_coef       0.0030(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997b)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4630
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0678
_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^)+(0.101P)^2^+2.7759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                2771
_reflns_number_total             4630
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1108.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014645
_cod_database_fobs_code          2014645