Di-μ~2~-methoxo-bis{[μ-3,10,18,25-tetraazapentacyclo[17.4.4.3.1.1]triconta-1(31),2,4(9),5,7,10,12,14,16(32),17,19(24),20,22,25,27,29-hexadecaene-31,32-diolato]dizinc(II)} bis(perchlorate) <i>N</i>,<i>N</i>-dimethylformamide disolvate
Lim, Zelong; Forsyth, Craig M.; Graham, Bim; Acta Crystallographica Section E 67 (2011) m368–; doi:10.1107/S1600536811005873

data_2229412
_publ_section_title
;
 Di-\m~2~-methoxo-bis{[\m-3,10,18,25-tetraazapentacyclo[17.4.4.3.1.1]triconta-1(31),2,4(9),5,7,10,12,14,16(32),17,19(24),20,22,25,27,29-hexadecaene-31,32-diolato]dizinc(II)}
 bis(perchlorate) <i>N</i>,<i>N</i>-dimethylformamide disolvate
;
_journal_coeditor_code           IM2265
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m368
_journal_paper_doi               10.1107/S1600536811005873
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Zn4 (C28 H18 N4 O2)2 (C H3 O)2] (Cl O4)2, 2C3 H7 N O'
_chemical_formula_moiety
'C58 H42 N8 O6 Zn4 2+, 2(Cl O4 -), 2(C3 H7 N O)'
_chemical_formula_sum            'C64 H56 Cl2 N10 O16 Zn4'
_chemical_formula_weight         1553.57
_chemical_name_systematic
;
Di-\m~2~-methoxo-bis{[\m-3,10,18,25-tetraazapentacyclo[17.4.4.3.1.1]triconta-
1(31),2,4(9),5,7,10,12,14,16(32),17,19(24),20,22,25,27,29-hexadecaene-31,32-
diolato]dizinc(II)} bis(perchlorate) <i>N</i>,<i>N</i>-dimethylformamide
disolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.0190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.9454(4)
_cell_length_b                   10.4512(2)
_cell_length_c                   20.5774(4)
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.07
_cell_volume                     6169.65(19)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2004)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin-slice \f and \w'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32276
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6063
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0611P)^2^+14.7497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                4245
_reflns_number_total             6063
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2265.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2229412
_cod_database_fobs_code          2229412