#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:02:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179773 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/69/7006930.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7006930
loop_
_publ_author_name
'Cingolani, Augusto'
'Galli, Simona'
'Masciocchi, Norberto'
'Pandolfo, Luciano'
'Pettinari, Claudio'
'Sironi, Angelo'
_publ_section_title
;
 The competition between acetate and pyrazolate in the formation of
 polynuclear Zn(II) coordination complexes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2479
_journal_page_last               2486
_journal_paper_doi               10.1039/b515630k
_journal_year                    2006
_chemical_formula_moiety         'C16 H20 N8 O4 Zn2'
_chemical_formula_sum            'C16 H20 N8 O4 Zn2'
_chemical_formula_weight         519.04
_chemical_name_systematic
;
bis-pyrazole bis-mu-pyrazolate bis-acetato dizinc(ii)
;
_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                105.22(3)
_cell_angle_beta                 106.98(3)
_cell_angle_gamma                103.84(4)
_cell_formula_units_Z            1
_cell_length_a                   8.197(4)
_cell_length_b                   8.300(4)
_cell_length_c                   9.256(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     546.1(5)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        local
_computing_molecular_graphics    WINGX
_computing_publication_material  CIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_method       omega-scan
_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  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2100
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 14400
_diffrn_standards_interval_time  300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0518P)²+0.1251P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                1682
_reflns_number_total             1969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b515630k.txt
_cod_data_source_block           Compound_1
_cod_original_cell_volume        546.1(4)
_cod_database_code               7006930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.39110(5) 0.60181(5) 0.86850(4) 0.04562(15) Uani 1 1 d . . .
O1 O 0.4802(3) 0.7065(3) 0.7284(3) 0.0587(6) Uani 1 1 d . . .
O2 O 0.2044(3) 0.5565(4) 0.5506(3) 0.0677(7) Uani 1 1 d . . .
N1 N 0.3384(3) 0.3441(3) 0.8099(3) 0.0458(6) Uani 1 1 d . . .
N2 N 0.4124(4) 0.2671(3) 0.9130(3) 0.0501(7) Uani 1 1 d . . .
N3 N 0.1808(4) 0.6722(4) 0.8989(3) 0.0483(6) Uani 1 1 d . . .
N4 N 0.0208(4) 0.6394(4) 0.7844(3) 0.0554(7) Uani 1 1 d . . .
H4n H -0.0083 0.5850 0.6828 0.067 Uiso 1 1 calc R . .
C1 C 0.2187(5) 0.2141(5) 0.6743(4) 0.0607(9) Uani 1 1 d . . .
H1 H 0.1495 0.2307 0.5836 0.073 Uiso 1 1 calc R . .
C2 C 0.2116(5) 0.0522(5) 0.6871(5) 0.0676(10) Uani 1 1 d . . .
H2 H 0.1387 -0.0597 0.6103 0.081 Uiso 1 1 calc R . .
C3 C 0.3350(5) 0.0917(5) 0.8370(5) 0.0675(11) Uani 1 1 d . . .
H3 H 0.3618 0.0080 0.8808 0.081 Uiso 1 1 calc R . .
C4 C 0.1696(5) 0.7572(5) 1.0361(5) 0.0649(10) Uani 1 1 d . . .
H4 H 0.2621 0.7979 1.1375 0.078 Uiso 1 1 calc R . .
C5 C 0.0029(6) 0.7771(6) 1.0088(6) 0.0806(13) Uani 1 1 d . . .
H5 H -0.0385 0.8312 1.0854 0.097 Uiso 1 1 calc R . .
C6 C -0.0879(5) 0.7016(6) 0.8475(6) 0.0732(11) Uani 1 1 d . . .
H6 H -0.2052 0.6943 0.7906 0.088 Uiso 1 1 calc R . .
C7 C 0.3582(5) 0.6583(5) 0.5900(4) 0.0532(8) Uani 1 1 d . . .
C8 C 0.4113(7) 0.7347(7) 0.4745(6) 0.0884(14) Uani 1 1 d . . .
H8A H 0.5361 0.8110 0.5257 0.133 Uiso 0.50 1 calc PR . .
H8B H 0.3360 0.8019 0.4433 0.133 Uiso 0.50 1 calc PR . .
H8C H 0.3960 0.6402 0.3803 0.133 Uiso 0.50 1 calc PR . .
H8D H 0.3093 0.6910 0.3738 0.133 Uiso 0.50 1 calc PR . .
H8E H 0.5094 0.7002 0.4562 0.133 Uiso 0.50 1 calc PR . .
H8F H 0.4494 0.8619 0.5192 0.133 Uiso 0.50 1 calc PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn 0.0406(2) 0.0478(2) 0.0466(2) 0.01614(16) 0.01088(15) 0.01973(16)
O1 0.0496(13) 0.0700(16) 0.0572(15) 0.0265(12) 0.0178(12) 0.0205(12)
O2 0.0513(15) 0.094(2) 0.0525(14) 0.0260(14) 0.0185(12) 0.0180(14)
N1 0.0411(14) 0.0457(14) 0.0430(14) 0.0107(12) 0.0098(11) 0.0155(11)
N2 0.0460(15) 0.0402(14) 0.0528(16) 0.0110(12) 0.0062(12) 0.0170(12)
N3 0.0455(14) 0.0599(17) 0.0435(14) 0.0182(13) 0.0169(12) 0.0251(13)
N4 0.0472(15) 0.0670(18) 0.0506(16) 0.0180(14) 0.0125(13) 0.0277(14)
C1 0.055(2) 0.060(2) 0.0448(19) 0.0100(16) 0.0036(16) 0.0098(17)
C2 0.057(2) 0.048(2) 0.064(2) -0.0034(17) 0.0064(18) 0.0055(16)
C3 0.059(2) 0.0441(19) 0.083(3) 0.0162(19) 0.008(2) 0.0194(17)
C4 0.067(2) 0.080(3) 0.048(2) 0.0156(18) 0.0242(18) 0.030(2)
C5 0.080(3) 0.093(3) 0.080(3) 0.018(2) 0.049(3) 0.041(3)
C6 0.049(2) 0.088(3) 0.090(3) 0.029(2) 0.030(2) 0.036(2)
C7 0.055(2) 0.065(2) 0.051(2) 0.0244(17) 0.0257(17) 0.0301(18)
C8 0.101(3) 0.103(4) 0.075(3) 0.048(3) 0.045(3) 0.027(3)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn N1 115.60(11) . . ?
O1 Zn N2 103.94(12) . 2_667 ?
N1 Zn N2 110.66(11) . 2_667 ?
O1 Zn N3 111.41(11) . . ?
N1 Zn N3 111.85(12) . . ?
N2 Zn N3 102.25(11) 2_667 . ?
C7 O1 Zn 111.7(2) . . ?
C1 N1 N2 107.4(3) . . ?
C1 N1 Zn 128.5(2) . . ?
N2 N1 Zn 123.87(19) . . ?
C3 N2 N1 107.2(3) . . ?
C3 N2 Zn 127.7(2) . 2_667 ?
N1 N2 Zn 125.1(2) . 2_667 ?
C4 N3 N4 105.0(3) . . ?
C4 N3 Zn 127.7(2) . . ?
N4 N3 Zn 127.3(2) . . ?
C6 N4 N3 111.4(3) . . ?
N1 C1 C2 110.3(3) . . ?
C3 C2 C1 104.4(3) . . ?
N2 C3 C2 110.7(3) . . ?
N3 C4 C5 110.9(4) . . ?
C6 C5 C4 105.3(3) . . ?
N4 C6 C5 107.5(3) . . ?
O2 C7 O1 123.1(3) . . ?
O2 C7 C8 121.0(4) . . ?
O1 C7 C8 116.0(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn O1 1.952(3) . ?
Zn N1 1.967(3) . ?
Zn N2 1.993(3) 2_667 ?
Zn N3 2.017(3) . ?
O1 C7 1.262(4) . ?
O2 C7 1.223(4) . ?
N1 C1 1.329(4) . ?
N1 N2 1.362(4) . ?
N2 C3 1.333(4) . ?
N2 Zn 1.993(3) 2_667 ?
N3 C4 1.322(4) . ?
N3 N4 1.336(4) . ?
N4 C6 1.329(5) . ?
C1 C2 1.368(5) . ?
C2 C3 1.356(5) . ?
C4 C5 1.374(6) . ?
C5 C6 1.346(6) . ?
C7 C8 1.493(5) . ?
