Tetraaquatetrakis{μ~3~-3,3'-[(<i>E</i>,<i>E</i>)-ethane-1,2-diylbis(nitrilomethylidyne)]benzene-1,2-diolato}octazinc(II) <i>N</i>,<i>N</i>-dimethylformamide hexasolvate
Xu, Qin-Juan; Lin, Li-Rong; Sun, Di; Huang, Rong-Bin; Zheng, Lan-Sun; Acta Crystallographica Section E 65 (2009) m1559–m1560; doi:10.1107/S1600536809046923

data_2224434
_publ_section_title
;Tetraaquatetrakis{\m~3~-3,3'-[(<i>E</i>,<i>E</i>)-ethane-1,2-diylbis(nitrilomethylidyne)]benzene-1,2-diolato}octazinc(II)
 <i>N</i>,<i>N</i>-dimethylformamide hexasolvate
;
_journal_coeditor_code           SJ2663
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1559
_journal_page_last               m1560
_journal_paper_doi               10.1107/S1600536809046923
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Zn8 (C16 H12 N2 O4)4 (H2 O)4], 6C3 H7 N O'
_chemical_formula_moiety         'C64 H56 N8 O20 Zn8, 6(C3 H7 N O)'
_chemical_formula_sum            'C82 H98 N14 O26 Zn8'
_chemical_formula_weight         2218.69
_chemical_name_systematic
;
Tetraaquatetrakis{\m~3~-3,3'-[(<i>E</i>,<i>E</i>)-ethane-1,2-
diylbis(nitrilomethylidyne)]benzene-1,2-diolato}octazinc(II)
<i>N</i>,<i>N</i>-dimethylformamide hexasolvate
;
_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                80.599(2)
_cell_angle_beta                 76.519(2)
_cell_angle_gamma                72.734(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5451(4)
_cell_length_b                   14.2114(4)
_cell_length_c                   25.0620(6)
_cell_measurement_reflns_used    28634
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.5604
_cell_measurement_theta_min      2.2383
_cell_volume                     4456.9(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S Ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51671
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.379
_refine_ls_extinction_coef       0.00041(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1184
_refine_ls_number_reflns         17430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                13557
_reflns_number_total             17430
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2663.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C82 H98 N14 O26 Zn8 '
_cod_database_code               2224434
_cod_database_fobs_code          2224434