One-Pot Template Synthesis and Properties of a Molecular Bowl: Dodecaaza Macrotetracycle with μ3-Oxo and μ3-Hydroxo Tricopper(II) Cores
Myunghyun Paik Suh; Mi Young Han; Jea Ho Lee; Kil Sik Min; Changbong Hyeon; Journal of the American Chemical Society 120 (1998) 3819–3820; doi:10.1021/ja9721780

data_4116716
_publ_section_title
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 One-Pot Template Synthesis and Properties of a Molecular Bowl: Dodecaaza
 Macrotetracycle with \m3-Oxo and \m3-Hydroxo Tricopper(II) Cores
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3819
_journal_page_last               3820
_journal_paper_doi               10.1021/ja9721780
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C24 H58 Cl4 Cu3 N12 O19'
_chemical_formula_weight         1151.24
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.443(3)
_cell_length_b                   20.443(3)
_cell_length_c                   20.443(3)
_cell_measurement_temperature    293(2)
_cell_volume                     8543(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6261
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.818
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_F_000             4744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+8.8773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1131
_refine_ls_wR_factor_obs         0.0927
_reflns_number_observed          2034
_reflns_number_total             3054
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9721780_1.cif
_cod_data_source_block           final
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+8.8773P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+8.8773P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8543.5(22)
_cod_database_code               4116716