#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/44/2014413.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_2014413
loop_
_publ_author_name
'Juan Granifo'
'María Teresa Garland'
'Ricardo Baggio'
_publ_section_title
;Two one-dimensional zinc(II) coordination polymers:
 catena-poly[[bis(pentane-2,4-dionato-κ²O,O')zinc]-μ-1,4-bis(x-pyridyl)-2,3-diazabuta-1,3-diene]
 (x = 3, 4)
;
_journal_coeditor_code           SQ3002
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m56
_journal_page_last               m59
_journal_paper_doi               10.1107/S0108270106000540
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Zn (C5 H7 O2)2 (C12 H10 N4)]'
_chemical_formula_moiety         'C22 H24 N4 O4 Zn '
_chemical_formula_sum            'C22 H24 N4 O4 Zn'
_chemical_formula_weight         473.82
_chemical_name_systematic
;
catena-poly[[bis(pentane-2,4-dionato-κ²O,O')zinc]-μ-
1,4-bis(3-pyridyl)-2,3-diazabuta-1,3-diene]
;
_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                80.536(3)
_cell_angle_beta                 73.444(3)
_cell_angle_gamma                77.310(3)
_cell_formula_units_Z            1
_cell_length_a                   6.8637(11)
_cell_length_b                   8.6257(14)
_cell_length_c                   9.9497(16)
_cell_measurement_reflns_used    1134
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      3.45
_cell_volume                     547.57(15)
_computing_cell_refinement       'SAINT-NT (Bruker, 2000)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        SAINT-NT
_computing_molecular_graphics    'XP in SHELXTL-PC (Sheldrick, 2000 or 1994?)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4661
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.309
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0540
_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)+(0.0584P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                1898
_reflns_number_total             2379
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3002.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2014413
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn1 0.5000 0.5000 0.5000 0.0371(2) Uani d S 1 . . Zn
C1 1.1023(5) 0.4043(4) 0.1656(3) 0.0376(7) Uani d . 1 . . C
C2 0.9477(5) 0.4470(4) 0.2834(3) 0.0395(8) Uani d . 1 . . C
H2 0.9710 0.5151 0.3383 0.047 Uiso calc R 1 . . H
N3 0.7661(4) 0.3971(3) 0.3243(3) 0.0384(6) Uani d . 1 . . N
C4 0.7409(5) 0.2940(4) 0.2471(4) 0.0433(8) Uani d . 1 . . C
H4 0.6169 0.2563 0.2737 0.052 Uiso calc R 1 . . H
C5 0.8884(5) 0.2404(4) 0.1305(4) 0.0502(9) Uani d . 1 . . C
H5 0.8651 0.1660 0.0817 0.060 Uiso calc R 1 . . H
C6 1.0703(5) 0.2975(4) 0.0866(4) 0.0454(8) Uani d . 1 . . C
H6 1.1699 0.2656 0.0060 0.054 Uiso calc R 1 . . H
C7 1.2880(5) 0.4750(4) 0.1268(3) 0.0415(8) Uani d . 1 . . C
H7 1.3105 0.5334 0.1898 0.050 Uiso calc R 1 . . H
N8 1.4192(4) 0.4582(3) 0.0087(3) 0.0466(7) Uani d . 1 . . N
C9 0.3745(6) 0.8894(5) 0.1823(4) 0.0612(11) Uani d . 1 . . C
H9A 0.4270 0.8348 0.0991 0.092 Uiso calc R 1 . . H
H9B 0.4138 0.9926 0.1627 0.092 Uiso calc R 1 . . H
H9C 0.2265 0.9022 0.2108 0.092 Uiso calc R 1 . . H
C10 0.4627(5) 0.7930(4) 0.2992(3) 0.0435(8) Uani d . 1 . . C
C11 0.6128(5) 0.8480(4) 0.3381(4) 0.0500(9) Uani d . 1 . . C
H11 0.6565 0.9393 0.2853 0.060 Uiso calc R 1 . . H
C12 0.7044(5) 0.7812(4) 0.4475(4) 0.0416(8) Uani d . 1 . . C
C13 0.8543(6) 0.8638(5) 0.4792(5) 0.0592(11) Uani d . 1 . . C
H13A 0.8156 0.8759 0.5781 0.089 Uiso calc R 1 . . H
H13B 0.8523 0.9672 0.4258 0.089 Uiso calc R 1 . . H
H13C 0.9909 0.8012 0.4542 0.089 Uiso calc R 1 . . H
O14 0.6730(3) 0.6523(3) 0.5243(2) 0.0412(6) Uani d . 1 . . O
O15 0.3908(3) 0.6683(3) 0.3550(2) 0.0423(6) Uani d . 1 . . O
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_3
_geom_angle
_geom_angle_publ_flag
O14 Zn1 O14 2_666 180.0 ?
O14 Zn1 O15 . 89.49(9) y
O14 Zn1 O15 2_666 90.51(9) ?
O15 Zn1 O15 2_666 180.00(9) ?
O14 Zn1 N3 . 90.04(9) y
O14 Zn1 N3 2_666 89.96(9) ?
O15 Zn1 N3 . 89.88(9) ?
O15 Zn1 N3 2_666 90.12(9) ?
O14 Zn1 N3 2_666 89.96(9) ?
O14 Zn1 N3 . 90.04(9) ?
O15 Zn1 N3 2_666 90.12(9) ?
O15 Zn1 N3 . 89.88(9) y
N3 Zn1 N3 2_666 180.0 ?
C2 C1 C6 . 117.7(3) ?
C2 C1 C7 . 119.3(3) ?
C6 C1 C7 . 123.0(3) ?
N3 C2 C1 . 124.4(3) ?
N3 C2 H2 . 117.8 ?
C1 C2 H2 . 117.8 ?
C4 N3 C2 . 116.4(3) ?
C4 N3 Zn1 . 120.7(2) ?
C2 N3 Zn1 . 122.6(2) ?
N3 C4 C5 . 123.5(3) ?
N3 C4 H4 . 118.2 ?
C5 C4 H4 . 118.2 ?
C6 C5 C4 . 119.4(3) ?
C6 C5 H5 . 120.3 ?
C4 C5 H5 . 120.3 ?
C5 C6 C1 . 118.5(3) ?
C5 C6 H6 . 120.7 ?
C1 C6 H6 . 120.7 ?
N8 C7 C1 . 121.2(3) ?
N8 C7 H7 . 119.4 ?
C1 C7 H7 . 119.4 ?
C7 N8 N8 2_865 111.5(3) ?
C10 C9 H9A . 109.5 ?
C10 C9 H9B . 109.5 ?
H9A C9 H9B . 109.5 ?
C10 C9 H9C . 109.5 ?
H9A C9 H9C . 109.5 ?
H9B C9 H9C . 109.5 ?
O15 C10 C11 . 125.4(3) ?
O15 C10 C9 . 116.2(3) ?
C11 C10 C9 . 118.5(3) ?
C12 C11 C10 . 127.1(3) ?
C12 C11 H11 . 116.5 ?
C10 C11 H11 . 116.5 ?
O14 C12 C11 . 125.0(3) ?
O14 C12 C13 . 115.7(3) ?
C11 C12 C13 . 119.3(3) ?
C12 C13 H13A . 109.5 ?
C12 C13 H13B . 109.5 ?
H13A C13 H13B . 109.5 ?
C12 C13 H13C . 109.5 ?
H13A C13 H13C . 109.5 ?
H13B C13 H13C . 109.5 ?
C12 O14 Zn1 . 126.2(2) ?
C10 O15 Zn1 . 125.5(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 O14 2_666 2.037(2) n
Zn1 O14 . 2.037(2) y
Zn1 O15 2_666 2.049(2) n
Zn1 O15 . 2.049(2) y
Zn1 N3 2_666 2.271(3) n
Zn1 N3 . 2.271(3) y
C1 C2 . 1.378(4) ?
C1 C6 . 1.393(4) ?
C1 C7 . 1.459(4) ?
C2 N3 . 1.339(4) ?
C2 H2 . 0.9300 ?
N3 C4 . 1.334(4) ?
C4 C5 . 1.373(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.371(4) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 N8 . 1.268(4) ?
C7 H7 . 0.9300 ?
N8 N8 2_865 1.408(5) ?
C9 C10 . 1.508(5) ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 0.9600 ?
C10 O15 . 1.261(4) ?
C10 C11 . 1.393(5) ?
C11 C12 . 1.391(5) ?
C11 H11 . 0.9300 ?
C12 O14 . 1.264(4) ?
C12 C13 . 1.499(4) ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
