Novel Chiral "Calixsalen" Macrocycle and Chiral Robson-type Macrocyclic Complexes
Gao, Jian; Reibenspies, Joseph H.; Zingaro, Ralph A.; Woolley, F. Ross; Martell, Arthur E.; Clearfield, Abraham; Inorganic Chemistry 44 (2005) 232–241; doi:10.1021/ic049181m

data_4308425
_publ_section_title
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 Novel Chiral "Calixsalen" Macrocycle and Chiral Robson-type
 Macrocyclic Complexes
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_journal_coden_ASTM              INOCAJ
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              232
_journal_page_last               241
_journal_paper_doi               10.1021/ic049181m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C68 H91 Cl4 Co4 N8 O30'
_chemical_formula_weight         1878.01
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   16.970(5)
_cell_length_b                   19.821(5)
_cell_length_c                   23.093(5)
_cell_measurement_reflns_used    1385
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.23
_cell_volume                     7768(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.3445
_diffrn_reflns_av_sigmaI/netI    0.4737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41588
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.9008
_exptl_absorpt_correction_T_min  0.8149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3884
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.999
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_coef       0.0365(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         13474
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.3157
_refine_ls_R_factor_gt           0.0887
_refine_ls_shift/su_max          0.171
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.2350
_reflns_number_gt                3938
_reflns_number_total             13474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049181msi20040623_010730.cif
_cod_data_source_block           am168
_cod_depositor_comments
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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 
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_cod_database_code               4308425