Templating Schiff-Base Lateral Macrobicycles: An Experimental and Theoretical Structural Study of the Intermediates
Carlos Platas-Iglesias; David Esteban; Vicente Ojea; Fernando Avecilla; Andrés de Blas; Teresa Rodríguez-Blas; Inorganic Chemistry 42 (2003) 4299–4307; doi:10.1021/ic034266t

data_4313879
_publ_section_title
;
 Templating Schiff-Base Lateral Macrobicycles: An Experimental and
 Theoretical Structural Study of the Intermediates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4299
_journal_page_last               4307
_journal_paper_doi               10.1021/ic034266t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C26 H40 Ba Cl2 N4 O12'
_chemical_formula_weight         808.86
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                85.0750(10)
_cell_angle_beta                 80.9070(10)
_cell_angle_gamma                61.6270(10)
_cell_formula_units_Z            2
_cell_length_a                   10.467
_cell_length_b                   10.4755(2)
_cell_length_c                   16.9911(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1618.50(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10869
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  0.6294
_exptl_absorpt_correction_T_min  0.5293
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7715
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                5760
_reflns_number_total             7715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034266tsi20030311_120831_1.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1618.47(4)
_cod_database_code               4313879