6-Ammonio-(1<i>H</i>^+^)-1,4,8,11-tetraazacyclotridecane-5,7-dione Dichloride Methanol Solvate: an Amino-Pendant Tetraazacyclotridecane Derivative
Mishra, A. K.; Gestin, J. F.; Faivre-Chauvet, A.; Chatal, J. F.; Evain, M.; Acta Crystallographica Section C 52 (1996) 3100–3102; doi:10.1107/S0108270196009559

data_2005735
_publ_contact_author
;
      Michel Evain
      Laboratoire de Chimie des Solides
      I.M.N, UMR CNRS 110
      Universit\'e de Nantes
      2 Rue de la Houssini\`ere
      44072 Nantes
      France
;
_publ_section_title
;
 6-Ammonio-(1<i>H</i>^+^)-1,4,8,11-tetraazacyclotridecane-5,7-dione
 Dichloride Methanol Solvate: an Amino-Pendant Tetraazacyclotridecane
 Derivative
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              3100
_journal_page_last               3102
_journal_paper_doi               10.1107/S0108270196009559
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C9 H21 N5 O2 2+,2Cl -,C H4 O'
_chemical_formula_structural     'C9 H21 N5 O2 2+,2Cl -,C H4 O'
_chemical_formula_sum            'C10 H25 Cl2 N5 O3'
_chemical_formula_weight         334.2
_chemical_name_systematic
;
6-ammonio-1H^+^-1,4,8,11-tetraazacyclotridecane-5,7-dione
dichloride methanol solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                109.350(11)
_cell_angle_beta                 108.260(11)
_cell_angle_gamma                97.640(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0659(9)
_cell_length_b                   10.0897(10)
_cell_length_c                   10.4858(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     828.86(18)
_computing_data_collection       'CAD-4F Software (Enraf-Nonius, 1989)'
_computing_data_reduction        xtal_DIFDAT_ADDREF_ABSORB_SORTRF
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    'SHELXTL (Sheldrick, 1996)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf Nonius CAD4F'
_diffrn_measurement_method       \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  .021
_diffrn_reflns_av_sigmaI/netI    .073
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
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_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         39.99
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        25
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .41
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   xtal_ABSORB_gaussian
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallepiped
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.31
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_exptl_crystal_size_min          0.11
_refine_diff_density_max         .45
_refine_diff_density_min         -.31
_refine_ls_extinction_coef       0.047(2)
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_refine_ls_goodness_of_fit_obs   1.753
_refine_ls_hydrogen_treatment
'H atoms: refined freely with isotropic thermal parameters'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .040
_refine_ls_R_factor_obs          .040
_refine_ls_shift/esd_max         .001
_refine_ls_shift/esd_mean        .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F~o~^2^)+(0.019F~o~^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .052
_refine_ls_wR_factor_obs         .052
_reflns_number_observed          5943
_reflns_number_total             10248
_reflns_observed_criterion       refl_observed_if_F_>_4sigma(F)
_cod_data_source_file            bm1095.cif
_cod_data_source_block           BM1095
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Analytical' changed to
'analytical' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w =
1/[\s^2^(F~o~^2^)+(0.019F~o~^2^)]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(F~o~^2^)+(0.019F~o~^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        828.86(14)
_cod_database_code               2005735