#------------------------------------------------------------------------------
#$Date: 2016-01-22 05:57:28 +0200 (Fri, 22 Jan 2016) $
#$Revision: 174739 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/14/2241489.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241489
loop_
_publ_author_name
'Cai, Xue'
'Ning, Hui'
_publ_section_title
;
 Crystal structure of
 di-μ-acetato-diacetatobis(μ-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-μ-acetato-diacetatobis(μ-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/[σ²(Fo²)+(0.0367P)²+0.3975P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.5747(2) 0.1717(3) 0.1390(2) 0.0479(6) Uani d . 1 1
H H1A 0.5651 0.0938 0.1692 0.072 Uiso calc R 1 1
H H1B 0.5348 0.1350 0.0563 0.072 Uiso calc R 1 1
H H1C 0.5239 0.2186 0.1783 0.072 Uiso calc R 1 1
C C2 0.7601(2) 0.3909(2) 0.12186(18) 0.0334(4) Uani d . 1 1
C C3 0.6657(2) 0.4234(3) 0.0636(2) 0.0431(5) Uani d . 1 1
H H3 0.5666 0.3642 0.0497 0.052 Uiso calc R 1 1
C C4 0.7206(3) 0.5459(3) 0.0258(2) 0.0540(7) Uani d . 1 1
H H4 0.6577 0.5680 -0.0144 0.065 Uiso calc R 1 1
C C5 0.8656(3) 0.6339(3) 0.0473(2) 0.0485(6) Uani d . 1 1
H H5 0.9005 0.7136 0.0193 0.058 Uiso calc R 1 1
C C6 0.9640(2) 0.6057(2) 0.11148(18) 0.0344(5) Uani d . 1 1
C C7 0.9110(2) 0.4824(2) 0.14919(17) 0.0288(4) Uani d . 1 1
C C8 1.1149(2) 0.7072(2) 0.13321(19) 0.0374(5) Uani d . 1 1
H H8 1.1384 0.7791 0.0964 0.045 Uiso calc R 1 1
C C9 1.3647(2) 0.8311(2) 0.2054(2) 0.0428(5) Uani d . 1 1
H H9A 1.3563 0.9191 0.2172 0.051 Uiso calc R 1 1
H H9B 1.3959 0.8132 0.1316 0.051 Uiso calc R 1 1
C C10 1.4783(2) 0.8521(2) 0.3040(2) 0.0438(5) Uani d . 1 1
H H10A 1.4411 0.8567 0.3759 0.053 Uiso calc R 1 1
H H10B 1.5627 0.9436 0.3152 0.053 Uiso calc R 1 1
C C11 1.5238(3) 0.7346(3) 0.2830(2) 0.0503(6) Uani d . 1 1
H H11A 1.5415 0.7156 0.2039 0.060 Uiso calc R 1 1
H H11B 1.6138 0.7683 0.3370 0.060 Uiso calc R 1 1
C C12 1.4643(2) 0.5208(3) 0.33241(19) 0.0396(5) Uani d . 1 1
H H12 1.5642 0.5583 0.3466 0.048 Uiso calc R 1 1
C C13 1.3848(2) 0.3817(2) 0.35174(18) 0.0362(5) Uani d . 1 1
C C14 1.4677(3) 0.3186(3) 0.3880(2) 0.0446(6) Uani d . 1 1
H H14 1.5679 0.3689 0.4015 0.053 Uiso calc R 1 1
C C15 1.4038(3) 0.1858(3) 0.4035(2) 0.0499(6) Uani d . 1 1
H H15 1.4602 0.1465 0.4280 0.060 Uiso calc R 1 1
C C16 1.2532(3) 0.1083(3) 0.3828(2) 0.0435(5) Uani d . 1 1
H H16 1.2093 0.0169 0.3925 0.052 Uiso calc R 1 1
C C17 1.1699(2) 0.1679(2) 0.34775(18) 0.0354(5) Uani d . 1 1
C C18 1.2338(2) 0.3069(2) 0.33311(17) 0.0310(4) Uani d . 1 1
C C19 0.9443(3) -0.0457(3) 0.3169(3) 0.0661(8) Uani d . 1 1
H H19A 0.8425 -0.0761 0.2991 0.099 Uiso calc R 1 1
H H19B 0.9686 -0.0585 0.3910 0.099 Uiso calc R 1 1
H H19C 0.9691 -0.1021 0.2566 0.099 Uiso calc R 1 1
C C20 0.7933(2) -0.0082(2) 0.06099(19) 0.0343(4) Uani d . 1 1
C C21 0.7849(2) -0.1000(3) -0.0585(2) 0.0422(5) Uani d . 1 1
H H21A 0.7129 -0.1974 -0.0704 0.063 Uiso calc R 1 1
H H21B 0.8769 -0.0973 -0.0633 0.063 Uiso calc R 1 1
H H21C 0.7594 -0.0635 -0.1179 0.063 Uiso calc R 1 1
C C22 0.8649(2) 0.3057(2) 0.48569(18) 0.0314(4) Uani d . 1 1
C C23 1.0099(3) 0.3370(3) 0.5482(2) 0.0493(6) Uani d . 1 1
H H23A 1.0778 0.4354 0.5584 0.074 Uiso calc R 1 1
H H23B 1.0424 0.2747 0.5026 0.074 Uiso calc R 1 1
H H23C 1.0022 0.3208 0.6236 0.074 Uiso calc R 1 1
N N1 1.22093(19) 0.71044(18) 0.19729(15) 0.0340(4) Uani d . 1 1
N N2 1.41504(19) 0.59888(19) 0.29835(16) 0.0359(4) Uani d . 1 1
O O1 0.99395(15) 0.44590(15) 0.20882(13) 0.0329(3) Uani d . 1 1
O O2 1.14934(15) 0.35966(15) 0.30055(13) 0.0343(3) Uani d . 1 1
O O3 0.72225(16) 0.27149(18) 0.15849(17) 0.0488(4) Uani d . 1 1
O O4 1.02202(17) 0.10166(16) 0.32310(15) 0.0437(4) Uani d . 1 1
O O5 0.89752(18) 0.11959(17) 0.09127(14) 0.0436(4) Uani d . 1 1
O O6 0.7050(2) -0.0567(2) 0.12112(17) 0.0590(5) Uani d . 1 1
O O7 0.82953(16) 0.25334(17) 0.37574(13) 0.0409(4) Uani d . 1 1
O O8 0.77997(17) 0.33076(18) 0.54407(13) 0.0423(4) Uani d . 1 1
Zn Zn1 1.20447(2) 0.56385(2) 0.28798(2) 0.02906(8) Uani d . 1 1
Zn Zn2 0.92824(2) 0.25063(2) 0.24271(2) 0.02988(8) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 C1 H1A . . 109.5
O3 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
O3 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
O3 C2 C3 . . 125.4(2)
O3 C2 C7 . . 112.88(18)
C3 C2 C7 . . 121.7(2)
C2 C3 C4 . . 119.1(2)
C2 C3 H3 . . 120.4
C4 C3 H3 . . 120.4
C5 C4 C3 . . 120.6(2)
C5 C4 H4 . . 119.7
C3 C4 H4 . . 119.7
C4 C5 C6 . . 121.0(2)
C4 C5 H5 . . 119.5
C6 C5 H5 . . 119.5
C7 C6 C5 . . 119.1(2)
C7 C6 C8 . . 123.83(19)
C5 C6 C8 . . 117.1(2)
O1 C7 C6 . . 123.77(18)
O1 C7 C2 . . 117.92(17)
C6 C7 C2 . . 118.31(18)
N1 C8 C6 . . 127.81(19)
N1 C8 H8 . . 116.1
C6 C8 H8 . . 116.1
N1 C9 C10 . . 113.12(18)
N1 C9 H9A . . 109.0
C10 C9 H9A . . 109.0
N1 C9 H9B . . 109.0
C10 C9 H9B . . 109.0
H9A C9 H9B . . 107.8
C9 C10 C11 . . 114.1(2)
C9 C10 H10A . . 108.7
C11 C10 H10A . . 108.7
C9 C10 H10B . . 108.7
C11 C10 H10B . . 108.7
H10A C10 H10B . . 107.6
N2 C11 C10 . . 113.20(19)
N2 C11 H11A . . 108.9
C10 C11 H11A . . 108.9
N2 C11 H11B . . 108.9
C10 C11 H11B . . 108.9
H11A C11 H11B . . 107.8
N2 C12 C13 . . 128.7(2)
N2 C12 H12 . . 115.7
C13 C12 H12 . . 115.7
C18 C13 C14 . . 119.5(2)
C18 C13 C12 . . 123.98(19)
C14 C13 C12 . . 116.5(2)
C15 C14 C13 . . 121.3(2)
C15 C14 H14 . . 119.3
C13 C14 H14 . . 119.3
C14 C15 C16 . . 120.0(2)
C14 C15 H15 . . 120.0
C16 C15 H15 . . 120.0
C17 C16 C15 . . 119.8(2)
C17 C16 H16 . . 120.1
C15 C16 H16 . . 120.1
O4 C17 C16 . . 125.1(2)
O4 C17 C18 . . 113.64(18)
C16 C17 C18 . . 121.3(2)
O2 C18 C13 . . 122.92(19)
O2 C18 C17 . . 118.95(19)
C13 C18 C17 . . 118.12(19)
O4 C19 H19A . . 109.5
O4 C19 H19B . . 109.5
H19A C19 H19B . . 109.5
O4 C19 H19C . . 109.5
H19A C19 H19C . . 109.5
H19B C19 H19C . . 109.5
O6 C20 O5 . . 124.8(2)
O6 C20 C21 . . 120.8(2)
O5 C20 C21 . . 114.42(19)
C20 C21 H21A . . 109.5
C20 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
C20 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
O8 C22 O7 . . 120.8(2)
O8 C22 C23 . . 119.36(19)
O7 C22 C23 . . 119.80(19)
C22 C23 H23A . . 109.5
C22 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C22 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
C8 N1 C9 . . 115.46(18)
C8 N1 Zn1 . . 125.35(15)
C9 N1 Zn1 . . 119.19(14)
C12 N2 C11 . . 116.01(19)
C12 N2 Zn1 . . 124.81(15)
C11 N2 Zn1 . . 118.53(15)
C7 O1 Zn1 . . 129.06(12)
C7 O1 Zn2 . . 125.64(12)
Zn1 O1 Zn2 . . 105.29(6)
C18 O2 Zn2 . . 127.10(13)
C18 O2 Zn1 . . 129.24(13)
Zn2 O2 Zn1 . . 103.62(6)
C2 O3 C1 . . 119.07(18)
C2 O3 Zn2 . . 113.52(12)
C1 O3 Zn2 . . 127.31(14)
C17 O4 C19 . . 119.41(19)
C20 O5 Zn2 . . 120.25(14)
C22 O7 Zn2 . . 137.14(14)
C22 O8 Zn1 . 2_766 135.32(15)
O1 Zn1 O8 . 2_766 109.18(6)
O1 Zn1 N2 . . 149.75(7)
O8 Zn1 N2 2_766 . 98.57(7)
O1 Zn1 O2 . . 75.35(5)
O8 Zn1 O2 2_766 . 100.83(6)
N2 Zn1 O2 . . 88.08(6)
O1 Zn1 N1 . . 88.64(6)
O8 Zn1 N1 2_766 . 103.96(7)
N2 Zn1 N1 . . 96.30(7)
O2 Zn1 N1 . . 153.84(7)
O5 Zn2 O7 . . 137.44(7)
O5 Zn2 O2 . . 104.92(7)
O7 Zn2 O2 . . 110.70(6)
O5 Zn2 O1 . . 103.31(7)
O7 Zn2 O1 . . 107.96(6)
O2 Zn2 O1 . . 74.53(5)
O5 Zn2 O3 . . 85.68(7)
O7 Zn2 O3 . . 79.46(6)
O2 Zn2 O3 . . 143.50(5)
O1 Zn2 O3 . . 69.03(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O3 . 1.412(3)
C1 H1A . 0.9600
C1 H1B . 0.9600
C1 H1C . 0.9600
C2 O3 . 1.362(3)
C2 C3 . 1.378(3)
C2 C7 . 1.416(3)
C3 C4 . 1.394(3)
C3 H3 . 0.9300
C4 C5 . 1.363(4)
C4 H4 . 0.9300
C5 C6 . 1.417(3)
C5 H5 . 0.9300
C6 C7 . 1.399(3)
C6 C8 . 1.441(3)
C7 O1 . 1.325(2)
C8 N1 . 1.285(3)
C8 H8 . 0.9300
C9 N1 . 1.482(3)
C9 C10 . 1.514(3)
C9 H9A . 0.9700
C9 H9B . 0.9700
C10 C11 . 1.515(4)
C10 H10A . 0.9700
C10 H10B . 0.9700
C11 N2 . 1.479(3)
C11 H11A . 0.9700
C11 H11B . 0.9700
C12 N2 . 1.284(3)
C12 C13 . 1.452(3)
C12 H12 . 0.9300
C13 C18 . 1.402(3)
C13 C14 . 1.415(3)
C14 C15 . 1.359(4)
C14 H14 . 0.9300
C15 C16 . 1.398(4)
C15 H15 . 0.9300
C16 C17 . 1.382(3)
C16 H16 . 0.9300
C17 O4 . 1.370(3)
C17 C18 . 1.414(3)
C18 O2 . 1.322(2)
C19 O4 . 1.418(3)
C19 H19A . 0.9600
C19 H19B . 0.9600
C19 H19C . 0.9600
C20 O6 . 1.226(3)
C20 O5 . 1.277(3)
C20 C21 . 1.509(3)
C21 H21A . 0.9600
C21 H21B . 0.9600
C21 H21C . 0.9600
C22 O8 . 1.253(2)
C22 O7 . 1.259(2)
C22 C23 . 1.501(3)
C23 H23A . 0.9600
C23 H23B . 0.9600
C23 H23C . 0.9600
N1 Zn1 . 2.0727(17)
N2 Zn1 . 2.0616(18)
O1 Zn1 . 2.0203(14)
O1 Zn2 . 2.0639(14)
O2 Zn2 . 2.0632(14)
O2 Zn1 . 2.0676(14)
O3 Zn2 . 2.4356(16)
O5 Zn2 . 1.9261(15)
O7 Zn2 . 1.9635(14)
O8 Zn1 2_766 2.0201(15)
Zn1 O8 2_766 2.0201(15)

_cod_database_fobs_code 2241489
