The salt-type 1:2 adduct of <i>meso</i>-5,5,7,12,12,14-hexa-<i>C</i>-methyl-1,4,8,11-tetraazacyclotetradecane (tet-a) and 5-nitroisophthalic acid forms a hydrogen-bonded sheet structure containing two configurational isomers of [(tet-a)H~2~]^2+^
MacLean, Elizabeth J.; Teat, Simon J.; Farrell, Dorcas M. M.; Ferguson, George; Glidewell, Christopher; Acta Crystallographica Section C 58 (2002) o470–o473; doi:10.1107/S0108270102010958

data_2012910
_publ_section_title
;The salt-type 1:2 adduct of
 <i>meso</i>-5,5,7,12,12,14-hexa-<i>C</i>-methyl-1,4,8,11-tetraazacyclotetradecane
 (tet-a) and 5-nitroisophthalic acid forms a hydrogen-bonded sheet structure
 containing two configurational isomers of [(tet-a)H~2~]^2+^
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o470
_journal_page_last               o473
_journal_paper_doi               10.1107/S0108270102010958
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C16 H38 N4 2+ , 2C8 H4 N O6 -'
_chemical_formula_moiety         'C16 H38 N4 2+ , 2C8 H4 N O6 -'
_chemical_formula_sum            'C32 H46 N6 O12'
_chemical_formula_weight         706.46
_chemical_name_systematic
;
meso-5,7,7,12,14,14-hexamethyl-4,11-diaza-1,8-diazoniacyclotetradecane
bis(3-carboxy-5-nitrobenzoate)
;
_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
_cell_angle_alpha                66.6350(10)
_cell_angle_beta                 71.3870(10)
_cell_angle_gamma                82.9760(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5183(6)
_cell_length_b                   10.2278(8)
_cell_length_c                   11.3272(9)
_cell_measurement_reflns_used    5312
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.44
_cell_volume                     858.54(11)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'PLATON (Spek, 2002)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXTL and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6867
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8877
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.33
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4702
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.062
_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^)+(0.0776P)^2^+0.2773P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.160
_refine_ls_wR_factor_ref         0.165
_reflns_number_gt                4097
_reflns_number_total             4702
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tr1034.cif
_cod_data_source_block           I
_cod_depositor_comments
;
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_database_code               2012910
_cod_database_fobs_code          2012910