A neutral cubane with a Zn^II^~4~O~4~ core: tetrabenzoatotetrakis(μ~3~-hydroxydi-2-pyridylmethanolato)tetrazinc(II)‒acetone‒methanol (1/2/1)
Shin, Dong Hoon; Han, Sim-Hee; Kim, Pan-Gi; Kim, Cheal; Kim, Youngmee; Acta Crystallographica Section E 65 (2009) m658–m659; doi:10.1107/S1600536809017772

data_2222097
_publ_section_title
;A neutral cubane with a Zn^II^~4~O~4~ core:
 tetrabenzoatotetrakis(\m~3~-hydroxydi-2-pyridylmethanolato)tetrazinc(II)--acetone--methanol
 (1/2/1)
;
_journal_coeditor_code           LH2815
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m658
_journal_page_last               m659
_journal_paper_doi               10.1107/S1600536809017772
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Zn4 (C11 H9 N2 O2)4 (C7 H5 O2)4], 2C3 H6 O, C H4 O'
_chemical_formula_moiety         'C72 H56 N8 O16 Zn4, 2(C3 H6 O), C H4 O'
_chemical_formula_sum            'C316 H288 N32 O76 Zn16'
_chemical_formula_weight         6795.70
_chemical_name_systematic
;
Tetrabenzoatotetrakis(\m~3~-hydroxydi-2-pyridylmethanolato)tetrazinc(II)--
acetone--methanol (1/2/1)
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   14.3201(4)
_cell_length_b                   14.3201(4)
_cell_length_c                   37.730(2)
_cell_measurement_reflns_used    8208
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.84
_cell_volume                     7737.1(5)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            22787
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.416
_refine_ls_abs_structure_details 'Flack (1983), 2045 Friedel pairs'
_refine_ls_abs_structure_Flack   0.002(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0787P)^2^+0.4409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                4279
_reflns_number_total             4628
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2815.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 'Tetragonal' changed to 'tetragonal'
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_database_code               2222097
_cod_database_fobs_code          2222097