#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/97/4509731.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4509731
loop_
_publ_author_name
'Croitor, Lilia'
'Coropceanu, Eduard B.'
'Jeanneau, Erwann'
'Dementiev, Igor V.'
'Goglidze, Tatiana I.'
'Chumakov, Yurii M.'
'Fonari, Marina S.'
_publ_section_title
;
 Anion-Induced Generation of Binuclear and Polymeric Cd(II) and Zn(II)
 Coordination Compounds with 4,4'-Bipyridine and Dioxime Ligands
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5233
_journal_paper_doi               10.1021/cg900746w
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety
'4(C2 O2 H3), 2(C6 H10 N2 O2), (C10 H8 N2), 2(H2 O), Zn2'
_chemical_formula_sum            'C30 H44 N6 O14 Zn2'
_chemical_formula_weight         843.45
_chemical_name_common
; 
bis[zinc di(acetate)(1,2-cyclohexanedionedioxime)(aqua)]
(mu2-4,4'-bipyridine)
;
_chemical_name_systematic
; 
bis[zinc di(acetate)(1,2-cyclohexanedionedioxime)(aqua)]
(mu2-4,4'-bipyridine)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.834(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.7394(14)
_cell_length_b                   11.1708(8)
_cell_length_c                   8.4956(6)
_cell_measurement_reflns_used    5459
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.407
_cell_volume                     1839.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo&Scalepack(Otwinowski&Minor1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2974
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.64
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0432
_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)+(0.0971P)²+0.4130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                1505
_reflns_number_total             1781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900746wsup1.cif
_cod_data_source_block           l1
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4509731
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Zn1 Zn 0.19816(2) 0.0000 0.16514(5) 0.0623(2) Uani 1 2 d S
O1 O 0.27872(15) 0.2385(2) 0.3464(3) 0.0889(7) Uani 1 1 d .
H1A H 0.2509 0.2643 0.2579 0.133 Uiso 1 1 calc R
O2 O 0.13525(12) 0.1263(2) 0.0081(3) 0.0785(6) Uani 1 1 d .
O3 O 0.18939(15) 0.3000(2) 0.0667(3) 0.0939(7) Uani 1 1 d .
N1 N 0.27484(13) 0.1157(2) 0.3476(3) 0.0687(6) Uani 1 1 d .
N2 N 0.12929(18) 0.0000 0.3134(4) 0.0628(8) Uani 1 2 d S
C1 C 0.32155(14) 0.0663(3) 0.4719(3) 0.0689(7) Uani 1 1 d .
C2 C 0.3747(2) 0.1349(4) 0.6098(4) 0.0971(12) Uani 1 1 d .
H2A H 0.4027 0.1811 0.5616 0.116 Uiso 1 1 calc R
H2B H 0.3515 0.1906 0.6593 0.116 Uiso 1 1 calc R
C3 C 0.4200(4) 0.0566(6) 0.7432(8) 0.216(4) Uani 1 1 d .
H3A H 0.4668 0.0802 0.7575 0.259 Uiso 1 1 calc R
H3B H 0.4129 0.0802 0.8457 0.259 Uiso 1 1 calc R
C4 C 0.14227(18) 0.2340(3) -0.0220(4) 0.0738(8) Uani 1 1 d .
C5 C 0.0907(2) 0.2865(4) -0.1788(5) 0.1073(13) Uani 1 1 d .
H5A H 0.0571 0.2268 -0.2352 0.161 Uiso 1 1 calc R
H5B H 0.1140 0.3130 -0.2521 0.161 Uiso 1 1 calc R
H5C H 0.0681 0.3532 -0.1496 0.161 Uiso 1 1 calc R
C6 C 0.0620(2) 0.0000 0.2211(5) 0.0855(15) Uani 1 2 d S
H6A H 0.0491 0.0000 0.1044 0.103 Uiso 1 2 calc SR
C7 C 0.0104(2) 0.0000 0.2885(5) 0.0807(14) Uani 1 2 d S
H7A H -0.0357 0.0000 0.2179 0.097 Uiso 1 2 calc SR
C8 C 0.02757(19) 0.0000 0.4612(5) 0.0591(9) Uani 1 2 d S
C9 C 0.0971(2) 0.0000 0.5575(5) 0.0690(10) Uani 1 2 d S
H8A H 0.1114 0.0000 0.6744 0.083 Uiso 1 2 calc SR
C10 C 0.1452(2) 0.0000 0.4796(5) 0.0688(10) Uani 1 2 d S
H10A H 0.1917 0.0000 0.5474 0.083 Uiso 1 2 calc SR
O1W O 0.2578(3) 0.0000 0.0123(6) 0.0915(11) Uani 1 2 d S
H1W H 0.279(2) 0.059(4) 0.003(6) 0.137 Uiso 1 1 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'
Zn Zn 0.2839 1.4301 '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'
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
O2 Zn1 O2 86.58(14) 6 .
O2 Zn1 O1W 88.63(12) 6 .
O2 Zn1 O1W 88.63(12) . .
O2 Zn1 N1 172.49(9) 6 .
O2 Zn1 N1 100.75(10) . .
O1W Zn1 N1 89.91(13) . .
O2 Zn1 N1 100.75(10) 6 6
O2 Zn1 N1 172.49(9) . 6
O1W Zn1 N1 89.91(13) . 6
N1 Zn1 N1 71.87(14) . 6
O2 Zn1 N2 88.86(9) 6 .
O2 Zn1 N2 88.86(9) . .
O1W Zn1 N2 176.56(15) . .
N1 Zn1 N2 92.88(10) . .
N1 Zn1 N2 92.88(10) 6 .
N1 O1 H1A 109.5 . .
C4 O2 Zn1 134.4(2) . .
C1 N1 O1 114.1(3) . .
C1 N1 Zn1 118.3(2) . .
O1 N1 Zn1 127.6(2) . .
C10 N2 C6 115.9(4) . .
C10 N2 Zn1 129.5(3) . .
C6 N2 Zn1 114.6(3) . .
N1 C1 C1 115.59(18) . 6
N1 C1 C2 123.7(3) . .
C1 C1 C2 120.7(2) 6 .
C3 C2 C1 112.8(4) . .
C3 C2 H2A 109.0 . .
C1 C2 H2A 109.0 . .
C3 C2 H2B 109.0 . .
C1 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C3 C3 C2 126.3(3) 6 .
C3 C3 H3A 105.7 6 .
C2 C3 H3A 105.7 . .
C3 C3 H3B 105.7 6 .
C2 C3 H3B 105.7 . .
H3A C3 H3B 106.2 . .
O3 C4 O2 124.8(3) . .
O3 C4 C5 117.7(3) . .
O2 C4 C5 117.4(3) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C6 C7 123.9(4) . .
N2 C6 H6A 118.0 . .
C7 C6 H6A 118.0 . .
C8 C7 C6 119.7(4) . .
C8 C7 H7A 120.2 . .
C6 C7 H7A 120.2 . .
C7 C8 C9 116.7(4) . .
C7 C8 C8 121.0(4) . 5_556
C9 C8 C8 122.3(4) . 5_556
C10 C9 C8 119.8(4) . .
C10 C9 H8A 120.1 . .
C8 C9 H8A 120.1 . .
N2 C10 C9 124.0(4) . .
N2 C10 H10A 118.0 . .
C9 C10 H10A 118.0 . .
Zn1 O1W H1W 121(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 2.058(2) 6
Zn1 O2 2.058(2) .
Zn1 O1W 2.088(4) .
Zn1 N1 2.202(3) .
Zn1 N1 2.202(3) 6
Zn1 N2 2.215(3) .
O1 N1 1.375(3) .
O1 H1A 0.8200 .
O2 C4 1.249(4) .
O3 C4 1.242(4) .
N1 C1 1.277(4) .
N2 C10 1.331(5) .
N2 C6 1.336(5) .
C1 C1 1.481(7) 6
C1 C2 1.502(4) .
C2 C3 1.474(7) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C3 1.266(13) 6
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.500(5) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.382(6) .
C6 H6A 0.9300 .
C7 C8 1.381(6) .
C7 H7A 0.9300 .
C8 C9 1.382(6) .
C8 C8 1.510(8) 5_556
C9 C10 1.380(6) .
C9 H8A 0.9300 .
C10 H10A 0.9300 .
O1W H1W 0.81(5) .
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 H1W O3 0.81(5) 1.88(5) 2.676(3) 167(5) 7
O1 H1A O3 0.82 1.72 2.533(4) 172.8 .
