A barium perchlorate complex with a lateral macrobicycle derived from 4,13-diaza-18-crown-6 containing a pyridine Schiff base spacer
Avecilla, Fernando; Esteban, David; Platas-Iglesias, Carlos; Fernández-Martínez, Susana; De Blas, Andres; Rodríguez-Blas, Teresa; Acta Crystallographica Section C 59 (2003) m450–m451; doi:10.1107/S0108270103016901

data_2013637
_publ_section_title
;
 A barium perchlorate complex with a lateral macrobicycle derived from
 4,13-diaza-18-crown-6 containing a pyridine Schiff base spacer
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m450
_journal_page_last               m451
_journal_paper_doi               10.1107/S0108270103016901
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ba (Cl O4) (C33 H41 N5 O4)] (Cl O4)'
_chemical_formula_moiety         'C33 H41 Ba Cl N5 O8 + , Cl O4 -'
_chemical_formula_sum            'C33 H41 Ba Cl2 N5 O12'
_chemical_formula_weight         907.95
_chemical_name_systematic
;
(perchlorato-\k^2^O,O')[28,31,36,39-tetraoxa-1,9,17,25,42-
pentaazahexacyclo[23.8.5.1^11,15^.0^3,8^.0^18,23^]nonatriaconta-
3,5,7,9,11,13,15,16,18,20,22-undecane-
\k^8^N^1^,N^9^,N^17^,N^42^,O^28^,O^31^,O^36^,O^39^]barium(II) perchlorate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.6868(7)
_cell_length_b                   20.6923(8)
_cell_length_c                   20.7567(8)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.80
_cell_volume                     7596.5(5)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1997a)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \f-\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  0.062
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53172
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0.02
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         9421
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.093
_refine_ls_R_factor_gt           0.048
_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^)+(0.0141P)^2^+16.3465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.078
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                6140
_reflns_number_total             9421
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jz1570.cif
_cod_data_source_block           I
_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 
;
_cod_database_code               2013637
_cod_database_fobs_code          2013637