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_4308426
_publ_section_title
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 Novel Chiral "Calixsalen" Macrocycle and Chiral Robson-type
 Macrocyclic Complexes
;
_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            'C34.5 H43.5 N6 O4.75 Pb S2'
_chemical_formula_weight         889.56
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.814(4)
_cell_angle_beta                 67.952(4)
_cell_angle_gamma                88.071(4)
_cell_formula_units_Z            2
_cell_length_a                   11.593(3)
_cell_length_b                   12.366(3)
_cell_length_c                   14.880(4)
_cell_measurement_temperature    110(2)
_cell_volume                     1816.2(8)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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
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_diffrn_reflns_av_R_equivalents  0.0258
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_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15029
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    4.808
_exptl_absorpt_correction_T_max  0.4464
_exptl_absorpt_correction_T_min  0.4464
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             889
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(7)
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         11357
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                10369
_reflns_number_total             11357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049181msi20040623_010748.cif
_cod_data_source_block           am155
_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 
;
_cod_original_cell_volume        1816.3(8)
_cod_original_formula_sum        'C34.50 H43.50 N6 O4.75 Pb S2'
_cod_database_code               4308426