Crystal structure of di-μ-acetato-diacetatobis(μ-6,6'-dimethoxy-2,2'-{[(propane-1,3-diylbis(azanylylidene)]bis(methanylylidene)}diphenolato)tetrazinc
Cai, Xue; Ning, Hui; Acta Crystallographica Section E 71 (2015) m217–m218; doi:10.1107/S2056989015020551

data_2241489
_publ_section_title
;
 Crystal structure of
 di-\m-acetato-diacetatobis(\m-6,6'-dimethoxy-2,2'-{[(propane-1,3-diylbis(azanylylidene)]bis(methanylylidene)}diphenolato)tetrazinc
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m217
_journal_page_last               m218
_journal_paper_doi               10.1107/S2056989015020551
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Zn4 (C19 H20 N2 O4)2 (C2 H3 O2)4]'
_chemical_formula_moiety         'C46 H52 N4 O16 Zn4'
_chemical_formula_sum            'C46 H52 N4 O16 Zn4'
_chemical_formula_weight         1178.48
_chemical_name_systematic
Di-\m-acetato-diacetatobis(\m-6,6'-dimethoxy-2,2'-{[(propane-1,3-diylbis(azanylylidene)]bis(methanylylidene)}diphenolato)tetrazinc
_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                103.425(2)
_cell_angle_beta                 94.3230(10)
_cell_angle_gamma                115.6770(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4894(9)
_cell_length_b                   10.7917(9)
_cell_length_c                   11.9550(11)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.19
_cell_volume                     1162.17(18)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2001)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX 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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6281
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  0.8489
_exptl_absorpt_correction_T_min  0.7419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.3975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                3969
_reflns_number_total             4497
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pj2024sup1.cif
_cod_data_source_block           I
_cod_database_code               2241489
_cod_database_fobs_code          2241489