Unusual bridging of three nitrates with two bridgehead protons in an octaprotonated azacryptand.
Saeed, Musabbir A; Fronczek, Frank R; Huang, Ming-Ju; Alamgir Hossain, Md; Chemical communications (Cambridge, England) 46 (2010) 404–406; doi:10.1039/b923013k

data_7105166
_publ_section_title
;
 Unusual bridging of three nitrates with two bridgehead protons in an
 octaprotonated azacryptand.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              404
_journal_page_last               406
_journal_paper_doi               10.1039/b923013k
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C30 H56 N8 S3, 8(N O3), H N O3, 6(H2 O)'
_chemical_formula_sum            'C30 H69 N17 O33 S3'
_chemical_formula_weight         1292.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 106.553(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.394(2)
_cell_length_b                   13.713(2)
_cell_length_c                   23.772(3)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     5435.2(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       '\w and \f scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40019
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.07
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_refine_ls_extinction_method     none
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_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.128
_refine_ls_R_factor_gt           0.088
_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^)+(0.1553P)^2^+1.6394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.243
_refine_ls_wR_factor_ref         0.278
_reflns_number_gt                6444
_reflns_number_total             9562
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b923013k.txt
_cod_data_source_block           THEACRNO3
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7105166