#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/97/4509732.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_4509732
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
'Cd2, 4(C2 O2 H3), 2(C6 H10 N2 O2), (C10 H8 N2), 2(H2 O)'
_chemical_formula_sum            'C30 H44 Cd2 N6 O14'
_chemical_formula_weight         937.51
_chemical_name_common
; 
 bis[cadmium di(acetate)(1,2-cyclohexanedionedioxime)(aqua)]
(mu2-4,4'-bipyridine)
;
_chemical_name_systematic
; 
 bis[cadmium 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                 112.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.723(4)
_cell_length_b                   11.121(2)
_cell_length_c                   8.5449(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1913.6(7)
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius kappa CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_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            3291
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0047(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0401
_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)+(0.0519P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                1439
_reflns_number_total             1871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900746wsup1.cif
_cod_data_source_block           l3n
_cod_original_cell_volume        1913.6(6)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4509732
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.192340(19) 0.0000 0.15966(5) 0.0617(2) Uani 1 2 d S . .
O1 O 0.28111(18) 0.2412(3) 0.3562(4) 0.0883(9) Uani 1 1 d . . .
H1A H 0.2549 0.2676 0.2663 0.132 Uiso 1 1 calc R . .
O2 O 0.12555(15) 0.1396(3) -0.0073(4) 0.0840(9) Uani 1 1 d . . .
O3 O 0.19088(18) 0.2987(3) 0.0681(4) 0.0929(10) Uani 1 1 d . . .
N1 N 0.27653(16) 0.1183(3) 0.3566(4) 0.0655(9) Uani 1 1 d . . .
N2 N 0.1228(2) 0.0000 0.3198(5) 0.0647(12) Uani 1 2 d S . .
C1 C 0.32221(19) 0.0666(4) 0.4813(4) 0.0677(11) Uani 1 1 d . . .
C2 C 0.3747(2) 0.1352(5) 0.6182(5) 0.0923(16) Uani 1 1 d . . .
H1C2 H 0.3555 0.1704 0.6933 0.111 Uiso 0.50 1 calc PR A 1
H2C2 H 0.3909 0.2002 0.5683 0.111 Uiso 0.50 1 calc PR A 1
H3C2 H 0.3549 0.2049 0.6491 0.111 Uiso 0.50 1 d PR A 2
H4C2 H 0.4081 0.1633 0.5770 0.111 Uiso 0.50 1 d PR A 2
C3 C 0.4327(7) 0.0536(16) 0.7197(15) 0.123(7) Uani 0.50 1 d P . 1
H1C3 H 0.4695 0.0772 0.6882 0.148 Uiso 0.50 1 calc PR . 1
H2C3 H 0.4449 0.0772 0.8367 0.148 Uiso 0.50 1 calc PR . 1
C3* C 0.4080(6) 0.0539(15) 0.7768(12) 0.109(6) Uani 0.50 1 d P . 2
H1C4 H 0.4543 0.0780 0.8246 0.131 Uiso 0.50 1 calc PR . 2
H2C4 H 0.3888 0.0780 0.8577 0.131 Uiso 0.50 1 calc PR . 2
C4 C 0.1410(2) 0.2442(5) -0.0275(5) 0.0735(12) Uani 1 1 d . . .
C5 C 0.0950(3) 0.3095(6) -0.1833(6) 0.1079(18) Uani 1 1 d . . .
H5A H 0.0829 0.2566 -0.2789 0.162 Uiso 1 1 calc R . .
H5B H 0.1173 0.3788 -0.2038 0.162 Uiso 1 1 calc R . .
H5C H 0.0558 0.3346 -0.1659 0.162 Uiso 1 1 calc R . .
C6 C 0.1388(3) 0.0000 0.4847(7) 0.0696(16) Uani 1 2 d S . .
H6 H 0.1836 0.0000 0.5542 0.084 Uiso 1 2 calc SR . .
C7 C 0.0926(3) 0.0000 0.5587(7) 0.0697(16) Uani 1 2 d S . .
H7 H 0.1068 0.0000 0.6759 0.084 Uiso 1 2 calc SR . .
C8 C 0.0260(2) 0.0000 0.4636(6) 0.0555(13) Uani 1 2 d S . .
C9 C 0.0093(3) 0.0000 0.2911(7) 0.105(3) Uani 1 2 d S . .
H9 H -0.0350 0.0000 0.2183 0.125 Uiso 1 2 calc SR . .
C10 C 0.0596(3) 0.0000 0.2270(8) 0.123(4) Uani 1 2 d S . .
H10 H 0.0472 0.0000 0.1103 0.148 Uiso 1 2 calc SR . .
O1W O 0.2486(3) 0.0000 -0.0227(6) 0.0827(13) Uani 1 2 d S . .
H1W H 0.269(3) 0.070(5) -0.020(7) 0.124 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'
Cd Cd -0.8075 1.2024 '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 Cd1 O2 87.95(18) 6 .
O2 Cd1 O1W 87.16(13) 6 .
O2 Cd1 O1W 87.16(13) . .
O2 Cd1 N1 169.58(12) 6 .
O2 Cd1 N1 102.20(13) . .
O1W Cd1 N1 90.94(14) . .
O2 Cd1 N1 102.20(13) 6 6
O2 Cd1 N1 169.58(12) . 6
O1W Cd1 N1 90.94(14) . 6
N1 Cd1 N1 67.56(17) . 6
O2 Cd1 N2 88.11(11) 6 .
O2 Cd1 N2 88.11(11) . .
O1W Cd1 N2 173.43(16) . .
N1 Cd1 N2 94.53(12) . .
N1 Cd1 N2 94.53(12) 6 .
N1 O1 H1A 109.5 . .
C4 O2 Cd1 126.5(3) . .
C1 N1 O1 114.4(4) . .
C1 N1 Cd1 119.4(3) . .
O1 N1 Cd1 126.2(3) . .
C10 N2 C6 116.5(5) . .
C10 N2 Cd1 113.6(4) . .
C6 N2 Cd1 129.9(4) . .
N1 C1 C1 116.5(3) . 6
N1 C1 C2 122.8(4) . .
C1 C1 C2 120.6(3) 6 .
C1 C2 C3 111.3(7) . .
C1 C2 C3* 110.6(7) . .
C3 C2 C3* 31.9(5) . .
C1 C2 H1C2 109.4 . .
C3 C2 H1C2 109.4 . .
C3* C2 H1C2 80.4 . .
C1 C2 H2C2 109.4 . .
C3 C2 H2C2 109.4 . .
C3* C2 H2C2 133.2 . .
H1C2 C2 H2C2 108.0 . .
C1 C2 H3C2 109.5 . .
C3 C2 H3C2 132.4 . .
C3* C2 H3C2 109.5 . .
H1C2 C2 H3C2 32.0 . .
H2C2 C2 H3C2 78.3 . .
C1 C2 H4C2 109.5 . .
C3 C2 H4C2 80.0 . .
C3* C2 H4C2 109.5 . .
H1C2 C2 H4C2 132.6 . .
H2C2 C2 H4C2 32.3 . .
H3C2 C2 H4C2 108.1 . .
C3 C3 C2 126.4(6) 6 .
C3 C3 H1C3 105.7 6 .
C2 C3 H1C3 105.7 . .
C3 C3 H2C3 105.7 6 .
C2 C3 H2C3 105.7 . .
H1C3 C3 H2C3 106.2 . .
C3* C3* C2 125.3(6) 6 .
C3* C3* H1C4 106.0 6 .
C2 C3* H1C4 106.0 . .
C3* C3* H2C4 106.0 6 .
C2 C3* H2C4 106.0 . .
H1C4 C3* H2C4 106.3 . .
O2 C4 O3 125.5(4) . .
O2 C4 C5 116.6(5) . .
O3 C4 C5 117.9(5) . .
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 123.2(5) . .
N2 C6 H6 118.4 . .
C7 C6 H6 118.4 . .
C8 C7 C6 121.3(5) . .
C8 C7 H7 119.4 . .
C6 C7 H7 119.4 . .
C7 C8 C9 115.4(5) . .
C7 C8 C8 123.7(6) . 5_556
C9 C8 C8 120.9(6) . 5_556
C8 C9 C10 119.4(6) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N2 C10 C9 124.3(6) . .
N2 C10 H10 117.9 . .
C9 C10 H10 117.9 . .
Cd1 O1W H1W 111(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O2 2.235(3) 6
Cd1 O2 2.235(3) .
Cd1 O1W 2.313(4) .
Cd1 N1 2.366(3) .
Cd1 N1 2.366(3) 6
Cd1 N2 2.389(4) .
O1 N1 1.371(5) .
O1 H1A 0.8200 .
O2 C4 1.241(6) .
O3 C4 1.243(6) .
N1 C1 1.288(5) .
N2 C10 1.303(8) .
N2 C6 1.319(7) .
C1 C1 1.480(9) 6
C1 C2 1.500(6) .
C2 C3 1.532(17) .
C2 C3* 1.563(14) .
C2 H1C2 0.9700 .
C2 H2C2 0.9700 .
C2 H3C2 0.9700 .
C2 H4C2 0.9700 .
C3 C3 1.19(4) 6
C3 H1C3 0.9700 .
C3 H2C3 0.9700 .
C3* C3* 1.20(3) 6
C3* H1C4 0.9700 .
C3* H2C4 0.9700 .
C4 C5 1.517(6) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.373(8) .
C6 H6 0.9300 .
C7 C8 1.368(8) .
C7 H7 0.9300 .
C8 C9 1.380(7) .
C8 C8 1.479(10) 5_556
C9 C10 1.393(9) .
C9 H9 0.9300 .
C10 H10 0.9300 .
O1W H1W 0.89(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 0.89(5) 1.83(5) 2.697(4) 165(5) 7
O1 H1A O3 0.82 1.78 2.587(5) 169.5 .
