Adducts of <i>meso</i> and racemic 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane with trigonally trisubstituted benzene carboxylic acids: supramolecular structures in one and two dimensions
Burchell, Colin J.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section B 56 (2000) 1054–1062; doi:10.1107/S0108768100008302

data_2102195
_publ_section_title
;
 Adducts of <i>meso</i> and racemic
 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane with
 trigonally trisubstituted benzene carboxylic acids: supramolecular
 structures in one and two dimensions
;
_journal_coeditor_code           NA0108
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1054
_journal_page_last               1062
_journal_paper_doi               10.1107/S0108768100008302
_journal_volume                  56
_journal_year                    2000
_chemical_compound_source        'Synthesised by authors, see text'
_chemical_formula_moiety         'C16 H38 N4, 2(C7 H3 N2 O6)'
_chemical_formula_sum            'C30 H44 N8 O12'
_chemical_formula_weight         708.73
_chemical_name_systematic
;
 meso-5,5,7,12,12,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane--3,5-
dinitrobenzoic acid(1/2)

;
_space_group_IT_number           2
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                114.5800(17)
_cell_angle_beta                 91.9660(18)
_cell_angle_gamma                111.6740(18)
_cell_formula_units_Z            1
_cell_length_a                   8.7336(3)
_cell_length_b                   10.9388(3)
_cell_length_c                   11.0284(3)
_cell_measurement_reflns_used    12749
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.03
_cell_volume                     868.09(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'NRCVAX-96, ORTEP (Johnson, 1976), PLATON (Spek, 2000)'
_computing_publication_material
'NRCVAX-96, SHELXL-97  and WordPerfect macro PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'NRCVAX-96 and SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_l_max       15
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_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.106
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_exptl_absorpt_correction_T_min  0.9730
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
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_exptl_crystal_description       block
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_refine_ls_number_reflns         5013
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_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.1566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                3651
_reflns_number_total             5013
_reflns_threshold_expression     >2\s(I)
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_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 
;
_cod_original_cell_volume        868.09(4)
_cod_database_code               2102195