A barium perchlorate complex with a lateral macrobicycle derived from 1,10-diaza-15-crown-5 containing a phenol Schiff base spacer
Avecilla, Fernando; Esteban, David; Platas–Iglesias, Carlos; De Blas, Andres; Rodríguez–Blas, Teresa; Acta Crystallographica Section C 59 (2003) m93–m94; doi:10.1107/S0108270103002798

data_2013132
_publ_section_title
;
 A barium perchlorate complex with a lateral macrobicycle derived from
 1,10-diaza-15-crown-5 containing a phenol Schiff base spacer
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m93
_journal_page_last               m94
_journal_paper_doi               10.1107/S0108270103002798
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'C33 H40 Ba N4 O4, Cl O4, C2 H3 N, Cl O4, C H1.5, N0.5'
_chemical_formula_moiety
'C33 H40 Ba N4 O4, Cl O4, C2 H3 N, Cl O4, C H1.5, N0.5'
_chemical_formula_sum            'C36 H44.5 Ba Cl2 N5.5 O12'
_chemical_formula_weight         954.51
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                101.726(2)
_cell_angle_beta                 101.994(2)
_cell_angle_gamma                91.566(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5691(8)
_cell_length_b                   14.8261(13)
_cell_length_c                   15.7110(13)
_cell_measurement_reflns_used    14862
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.36
_cell_volume                     2129.2(3)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       '\f-\w scans'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14862
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        1.71
_diffrn_standards_number         '50 first frames'
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_T_max  0.6624
_exptl_absorpt_correction_T_min  0.5773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.558
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         10257
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0870P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                8410
_reflns_number_total             10257
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1006.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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_formula_sum        'C36 H44.50 Ba Cl2 N5.50 O12'
_cod_database_code               2013132
_cod_database_fobs_code          2013132