#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/00/1500035.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_1500035
loop_
_publ_author_name
'Carmen R. Maldonado'
'Miguel Quirós'
'Juan M. Salas'
_publ_contact_author_address
;
     Departamento de Química Inorgánica
     Facultad de Ciencias
     Universidad de Granada
     18071 Granada
     SPAIN
;
_publ_contact_author_email       mquiros@ugr.es
_publ_contact_author_fax         34-58-248526
_publ_contact_author_name        'Miguel Quirós'
_publ_contact_author_phone       34-58-240441
_journal_name_full               Polyhedron
_journal_page_first              911
_journal_page_last               916
_journal_paper_doi               10.1016/j.poly.2009.01.037
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C10 H18 N2 O4 Zn 2+, 2(C6 H6 N5 O2 1-)'
_chemical_formula_sum            'C22 H30 N12 O8 Zn'
_chemical_formula_weight         655.95
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.016(2)
_cell_angle_beta                 86.980(2)
_cell_angle_gamma                66.6810(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4090(9)
_cell_length_b                   8.9126(9)
_cell_length_c                   9.9452(10)
_cell_measurement_reflns_used    6128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.5
_cell_volume                     682.56(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'φ and ω 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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8018
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0.0
_diffrn_standards_number         234
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0240
_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/[σ²(Fo²)+(0.0300P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                3035
_reflns_number_total             3100
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dmaxpycompound5.cif
_cod_data_source_block           znpyrax
_cod_database_code               1500035
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 0.5000 0.5000 0.5000 0.01395(7) Uani 1 2 d S . .
N1P N 0.33922(14) 0.75519(14) 0.47032(11) 0.0163(2) Uani 1 1 d . . .
C2P C 0.36073(18) 0.86651(17) 0.54365(14) 0.0194(3) Uani 1 1 d . . .
H2P H 0.4426 0.8290 0.6134 0.023 Uiso 1 1 d R . .
C3P C 0.26912(19) 1.03315(17) 0.52258(14) 0.0211(3) Uani 1 1 d . . .
H3P H 0.2881 1.1080 0.5766 0.025 Uiso 1 1 d R . .
C4P C 0.14950(19) 1.08897(17) 0.42097(14) 0.0203(3) Uani 1 1 d . . .
H4P H 0.0854 1.2029 0.4039 0.024 Uiso 1 1 d R . .
C5P C 0.12477(18) 0.97564(17) 0.34504(14) 0.0200(3) Uani 1 1 d . . .
H5P H 0.0434 1.0104 0.2750 0.024 Uiso 1 1 d R . .
C6P C 0.22127(18) 0.81060(17) 0.37315(13) 0.0177(3) Uani 1 1 d . . .
H6P H 0.2032 0.7333 0.3215 0.021 Uiso 1 1 d R . .
N1 N 0.10472(15) 0.46536(14) 0.25822(11) 0.0161(2) Uani 1 1 d . . .
N2 N -0.05953(15) 0.49516(14) 0.29050(11) 0.0172(2) Uani 1 1 d . . .
N3 N -0.12883(14) 0.42388(14) 0.20585(11) 0.0163(2) Uani 1 1 d . . .
C3A C -0.00041(17) 0.34733(16) 0.11871(13) 0.0144(2) Uani 1 1 d . . .
N4 N -0.00465(14) 0.25630(14) 0.01425(11) 0.0156(2) Uani 1 1 d . . .
C4 C -0.16467(18) 0.23561(18) -0.01147(14) 0.0199(3) Uani 1 1 d . . .
H41 H -0.2101 0.2025 0.0730 0.024 Uiso 1 1 d R . .
H42 H -0.1401 0.1511 -0.0767 0.024 Uiso 1 1 d R . .
H43 H -0.2507 0.3393 -0.0480 0.024 Uiso 1 1 d R . .
C5 C 0.14028(17) 0.19054(16) -0.06818(13) 0.0158(3) Uani 1 1 d . . .
O5 O 0.14446(13) 0.11074(12) -0.16369(10) 0.0210(2) Uani 1 1 d . . .
N6 N 0.28849(14) 0.21754(14) -0.03625(11) 0.0159(2) Uani 1 1 d . . .
C6 C 0.43743(18) 0.15186(18) -0.13041(14) 0.0218(3) Uani 1 1 d . . .
H61 H 0.4165 0.2225 -0.2132 0.026 Uiso 1 1 d R . .
H62 H 0.4531 0.0413 -0.1523 0.026 Uiso 1 1 d R . .
H63 H 0.5420 0.1478 -0.0885 0.026 Uiso 1 1 d R . .
C7 C 0.30359(17) 0.30472(16) 0.07115(13) 0.0163(3) Uani 1 1 d . . .
O7 O 0.43992(13) 0.31864(13) 0.09108(10) 0.0223(2) Uani 1 1 d . . .
C7A C 0.14559(17) 0.37143(16) 0.14905(13) 0.0147(2) Uani 1 1 d . . .
O1W O 0.53138(12) 0.48345(12) 0.28531(10) 0.01728(19) Uani 1 1 d D . .
H11W H 0.487(2) 0.4391(19) 0.2370(15) 0.021 Uiso 1 1 d D . .
H12W H 0.6304(14) 0.467(2) 0.2531(17) 0.021 Uiso 1 1 d D . .
O2W O 0.28793(12) 0.43318(12) 0.49048(10) 0.01730(19) Uani 1 1 d D . .
H21W H 0.2110(18) 0.452(2) 0.5507(14) 0.021 Uiso 1 1 d D . .
H22W H 0.2277(19) 0.456(2) 0.4226(13) 0.021 Uiso 1 1 d D . .
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
O2W Zn O2W 180.0 . 2_666 ?
O2W Zn N1P 87.83(4) . 2_666 ?
O2W Zn N1P 92.17(4) 2_666 2_666 ?
O2W Zn N1P 92.17(4) . . ?
O2W Zn N1P 87.83(4) 2_666 . ?
N1P Zn N1P 180.0 2_666 . ?
O2W Zn O1W 88.09(4) . . ?
O2W Zn O1W 91.91(4) 2_666 . ?
N1P Zn O1W 90.85(4) 2_666 . ?
N1P Zn O1W 89.15(4) . . ?
O2W Zn O1W 91.91(4) . 2_666 ?
O2W Zn O1W 88.09(4) 2_666 2_666 ?
N1P Zn O1W 89.15(4) 2_666 2_666 ?
N1P Zn O1W 90.85(4) . 2_666 ?
O1W Zn O1W 180.0 . 2_666 ?
C2P N1P C6P 117.60(12) . . ?
C2P N1P Zn 120.63(9) . . ?
C6P N1P Zn 121.64(9) . . ?
N1P C2P C3P 123.10(13) . . ?
N1P C2P H2P 118.5 . . ?
C3P C2P H2P 118.4 . . ?
C2P C3P C4P 118.80(13) . . ?
C2P C3P H3P 120.6 . . ?
C4P C3P H3P 120.6 . . ?
C3P C4P C5P 118.83(13) . . ?
C3P C4P H4P 120.6 . . ?
C5P C4P H4P 120.6 . . ?
C6P C5P C4P 118.75(13) . . ?
C6P C5P H5P 120.6 . . ?
C4P C5P H5P 120.6 . . ?
N1P C6P C5P 122.91(12) . . ?
N1P C6P H6P 118.6 . . ?
C5P C6P H6P 118.5 . . ?
N2 N1 C7A 106.26(11) . . ?
N1 N2 N3 111.82(11) . . ?
C3A N3 N2 105.12(10) . . ?
N3 C3A N4 127.63(12) . . ?
N3 C3A C7A 109.41(11) . . ?
N4 C3A C7A 122.95(12) . . ?
C3A N4 C5 119.27(11) . . ?
C3A N4 C4 119.81(11) . . ?
C5 N4 C4 120.88(11) . . ?
N4 C4 H41 109.5 . . ?
N4 C4 H42 109.4 . . ?
H41 C4 H42 109.5 . . ?
N4 C4 H43 109.5 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
O5 C5 N4 122.64(12) . . ?
O5 C5 N6 120.36(12) . . ?
N4 C5 N6 116.99(11) . . ?
C7 N6 C5 126.73(11) . . ?
C7 N6 C6 118.06(11) . . ?
C5 N6 C6 115.16(11) . . ?
N6 C6 H61 109.5 . . ?
N6 C6 H62 109.4 . . ?
H61 C6 H62 109.5 . . ?
N6 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
O7 C7 N6 121.41(12) . . ?
O7 C7 C7A 126.40(12) . . ?
N6 C7 C7A 112.18(11) . . ?
N1 C7A C3A 107.39(11) . . ?
N1 C7A C7 130.78(12) . . ?
C3A C7A C7 121.82(12) . . ?
Zn O1W H11W 126.7(12) . . ?
Zn O1W H12W 116.0(12) . . ?
H11W O1W H12W 107.7(17) . . ?
Zn O2W H21W 123.1(12) . . ?
Zn O2W H22W 121.7(12) . . ?
H21W O2W H22W 100.0(17) . . ?
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 O2W 2.1000(10) . ?
Zn O2W 2.1001(10) 2_666 ?
Zn N1P 2.1453(11) 2_666 ?
Zn N1P 2.1453(11) . ?
Zn O1W 2.1456(10) . ?
Zn O1W 2.1456(10) 2_666 ?
N1P C2P 1.3437(17) . ?
N1P C6P 1.3448(17) . ?
C2P C3P 1.382(2) . ?
C2P H2P 0.9500 . ?
C3P C4P 1.386(2) . ?
C3P H3P 0.9500 . ?
C4P C5P 1.387(2) . ?
C4P H4P 0.9500 . ?
C5P C6P 1.386(2) . ?
C5P H5P 0.9500 . ?
C6P H6P 0.9500 . ?
N1 N2 1.3251(16) . ?
N1 C7A 1.3628(17) . ?
N2 N3 1.3679(16) . ?
N3 C3A 1.3353(17) . ?
C3A N4 1.3721(17) . ?
C3A C7A 1.3789(18) . ?
N4 C5 1.3772(17) . ?
N4 C4 1.4661(17) . ?
C4 H41 0.9800 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C5 O5 1.2166(16) . ?
C5 N6 1.4149(17) . ?
N6 C7 1.4030(17) . ?
N6 C6 1.4698(17) . ?
C6 H61 0.9800 . ?
C6 H62 0.9800 . ?
C6 H63 0.9800 . ?
C7 O7 1.2283(17) . ?
C7 C7A 1.4314(18) . ?
O1W H11W 0.830(9) . ?
O1W H12W 0.837(9) . ?
O2W H21W 0.832(9) . ?
O2W H22W 0.830(9) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O7 0.830(9) 2.007(10) 2.8153(14) 164.3(17) .
O1W H12W N3 0.837(9) 1.943(10) 2.7730(15) 171.5(17) 1_655
O2W H21W N2 0.832(9) 1.938(10) 2.7609(15) 169.9(17) 2_566
O2W H22W N1 0.830(9) 1.960(10) 2.7792(15) 169.3(17) .
