Structural studies of two protonated forms of a C2 symmetrical optically active cyclam derivative
Alfonso, Ignacio; Astorga, Covadonga; Rebolledo, Francisca; Gotor, Vicente; García-Granda, Santiago; Tesouro, Ana; Journal of the Chemical Society, Perkin Transactions 2  (2000) 899–; doi:10.1039/a904998c

data_7213177
_publ_section_title
;
 Structural studies of two protonated forms of a C2 symmetrical optically
 active cyclam derivative
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              899
_journal_paper_doi               10.1039/a904998c
_journal_year                    2000
_chemical_formula_moiety         'C14 H32 N4, (Cl O4)2'
_chemical_formula_sum            'C14 H32 Cl2 N4 O8'
_chemical_formula_weight         455.34
_chemical_name_systematic
; 

 2,6,9,13-tetraazabicyclo[12.4.0]octadecane-2,9-diium diperchlorate 

;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   'difference map and geometrical'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.01(6)
_cell_angle_beta                 94.67(5)
_cell_angle_gamma                116.89(7)
_cell_formula_units_Z            2
_cell_length_a                   8.033(6)
_cell_length_b                   8.268(7)
_cell_length_c                   18.029(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     1034.1(17)
_computing_cell_refinement       'CRYSDA (Beurskens et al, 1992)'
_computing_data_collection
;

 Nonius CAD4 Diffractometer Control Software. Data Collection with profile 

 analysis over all reflections. (Lehman and Larsen, 1974, Grant and Gable, 

 1978)

;
_computing_data_reduction        'THE REFLEX (local program)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material
;

 SHELXL-93 (Sheldrick, 1993). All calculations made at the University of 

Oviedo on the Scientific Computer Center and X-Ray group VAX/AXP computers. 

;
_computing_structure_refinement
;

 Anisotropic least-squares refinement carried out with SHELXL-93(Sheldrick, 

 1993). Geometricla calculations made with PARST (Nardelli, 1983).

;
_computing_structure_solution
;

 Direct methods using the SHELXS-86 (Sheldrick, 1990)

;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\Q
_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  0.0812
_diffrn_reflns_av_sigmaI/netI    0.2183
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3765
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.17
_diffrn_standards_decay_%        7.12
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   'XABS2 (Parkin et al,1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    'riding U isotropic commons'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.2101
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                1619
_reflns_number_total             3639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a904998csup1.cif
_cod_data_source_block           na294
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 'calc
w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1034.2(15)
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7213177