A 13-Membered Cyclic Tetraamine Salt: 12,12-Dimethyl-4,7,10-triaza-1-azoniacyclotridecane Perchlorate Hydrate
Gladkikh, Olga P.; Curtis, Neil F.; Turnbull, Mark M.; Acta Crystallographica Section C 53 (1997) 586–587; doi:10.1107/S0108270196015193

data_2006147
_publ_section_title
;
 A 13-Membered Cyclic Tetraamine Salt:
 12,12-Dimethyl-4,7,10-triaza-1-azoniacyclotridecane Perchlorate
 Hydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              586
_journal_page_last               587
_journal_paper_doi               10.1107/S0108270196015193
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C11 H27 N4 +,Cl O4 -,H2 O'
_chemical_formula_sum            'C11 H29 Cl N4 O5'
_chemical_formula_weight         332.83
_chemical_name_systematic
;3,3-Dimethyl-1,8,11-triaza-5-azoniumcyclotridecane
Perchlorate Water.
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.940(3)
_cell_length_b                   14.259(4)
_cell_length_c                   25.929(7)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      12.014
_cell_measurement_theta_min      4.759
_cell_volume                     3305.3(17)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XPMA (Zsolnai, 1994)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2563
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        4.23
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       'Rectangular block'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.264
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_method     'SHELXL-93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.878
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.878
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_obs          .0468
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(Fo^2^)+(0.0563P)^2^]
 where P = (Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.1115
_refine_ls_wR_factor_obs         .1039
_reflns_number_observed          1342
_reflns_number_total             2156
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1026.cif
_cod_data_source_block           13ane
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        3305(2)
_cod_database_code               2006147
_cod_database_fobs_code          2006147