#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:30:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179331 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322817.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_4322817
loop_
_publ_author_name
'Ming-Liang Tong'
'Bao-Hui Ye'
'Ji-Wen Cai'
'Xiao-Ming Chen'
'Seik Weng Ng'
_publ_contact_author
;
      Chen, Xiao-Ming
      Department of Chemistry
      Zhongshan University
      Guangzhou, 510275
      P. R. China
;
_publ_contact_author_email       cedc03@zsu.edu.cn
_publ_contact_author_fax         '86 20 4189173'
_publ_contact_author_phone       '86-20-84186300 ext 2074'
_publ_section_title
;
 Clathration of Two-Dimensional Coordination Polymers: Synthesis and
 Structures of [M(4,4'-bpy)₂](ClO₄)₂.(2,4'-bpy)₂.H₂O and
 [Cu(4,4'-bpy)₂(H₂O)₂](ClO₄)₄.(4,4'-H₂bpy) (M = CdII, ZnII
 and bpy = Bipyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2645
_journal_page_last               2650
_journal_paper_doi               10.1021/ic9714293
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C40 H38 Cl2 N8 O11 Zn'
_chemical_formula_weight         943.05
_chemical_name_systematic
; 
 'Bis(4,4'-bipyridine)diaqua-zinc(II) perchlorate bis(2,4'-bipyridine) aqua
solvate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.150(3)
_cell_length_b                   11.368(2)
_cell_length_c                   14.745(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.9
_cell_measurement_theta_min      8.2
_cell_volume                     2063.3(8)
_computing_cell_refinement       'CAD-4 VAX/PC (Enraf Nonius Delft, 1988)'
_computing_data_collection       'CAD-4 VAX/PC (Enraf Nonius Delft, 1988)'
_computing_data_reduction        'NRCVAX '
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω-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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3633
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.091
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_obs          0.0576
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1131P)²+1.3928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1660
_refine_ls_wR_factor_obs         0.1603
_reflns_number_observed          3192
_reflns_number_total             3633
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9714293_3.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+1.3928P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+1.3928P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2063.3(7)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4322817
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn 0.7500 0.02314(4) 0.7500 0.0219(2) Uani 1 d S .
N1 N 0.7500 -0.1643(3) 0.7500 0.0208(8) Uani 1 d S .
C11 C 0.7669(3) -0.2272(3) 0.8315(2) 0.0267(7) Uani 1 d . .
H11 H 0.7811(3) -0.1834(3) 0.8897(2) 0.080 Uiso 1 d R .
C12 C 0.7684(3) -0.3477(3) 0.8350(2) 0.0279(7) Uani 1 d . .
H12 H 0.7693(3) -0.3809(3) 0.8845(2) 0.080 Uiso 1 d R .
C13 C 0.7500 -0.4103(4) 0.7500 0.0217(9) Uani 1 d S .
C14 C 0.7500 -0.5426(4) 0.7500 0.0223(9) Uani 1 d S .
C15 C 0.8100(3) -0.6053(3) 0.8319(2) 0.0292(7) Uani 1 d . .
H15 H 0.8472(3) -0.5605(3) 0.8858(2) 0.080 Uiso 1 d R .
C16 C 0.8078(3) -0.7268(3) 0.8289(2) 0.0274(7) Uani 1 d . .
H16 H 0.8462(3) -0.7682(3) 0.8770(2) 0.080 Uiso 1 d R .
N2 N 0.7500 -0.7896(3) 0.7500 0.0199(8) Uani 1 d S .
N3 N 0.6582(2) 0.0174(2) 0.8489(2) 0.0265(6) Uani 1 d . .
O1W O 0.9025(2) 0.0197(2) 0.8741(2) 0.0315(6) Uani 1 d . .
H1WA H 0.9315(2) -0.0511(2) 0.8872(2) 0.080 Uiso 1 d R .
H1WB H 0.9437(2) 0.0834(2) 0.8779(2) 0.080 Uiso 1 d R .
C21 C 0.6879(3) 0.0721(3) 0.9349(3) 0.0338(8) Uani 1 d . .
H21 H 0.7361(3) 0.1294(3) 0.9416(3) 0.080 Uiso 1 d R .
C22 C 0.6280(3) 0.0686(4) 0.9947(3) 0.0390(9) Uani 1 d . .
H22 H 0.6591(3) 0.1098(4) 1.0527(3) 0.080 Uiso 1 d R .
C23 C 0.5324(3) 0.0037(3) 0.9683(3) 0.0268(7) Uani 1 d . .
C24 C 0.5032(3) -0.0533(4) 0.8798(3) 0.0396(9) Uani 1 d . .
H24 H 0.4451(3) -0.1065(4) 0.8657(3) 0.080 Uiso 1 d R .
C25 C 0.5663(3) -0.0442(4) 0.8232(3) 0.0381(9) Uani 1 d . .
H25 H 0.5565(3) -0.0919(4) 0.7659(3) 0.080 Uiso 1 d R .
N4 N 1.4351(3) 0.2925(4) 0.8741(4) 0.0726(14) Uani 1 d . .
N5 N 1.0768(3) 0.1644(4) 0.8874(3) 0.0514(9) Uani 1 d . .
C30 C 1.5195(5) 0.3504(6) 0.8663(6) 0.092(2) Uani 1 d . .
H30 H 1.5816(5) 0.3138(6) 0.8661(6) 0.080 Uiso 1 d R .
C31 C 1.5264(5) 0.4680(6) 0.8616(5) 0.081(2) Uani 1 d . .
H31 H 1.5782(5) 0.5109(6) 0.8446(5) 0.080 Uiso 1 d R .
C32 C 1.4415(5) 0.5322(5) 0.8648(5) 0.075(2) Uani 1 d . .
H32 H 1.4438(5) 0.6079(5) 0.8658(5) 0.080 Uiso 1 d R .
C33 C 1.3530(4) 0.4770(4) 0.8722(4) 0.0556(12) Uani 1 d . .
H33 H 1.2920(4) 0.5298(4) 0.8739(4) 0.080 Uiso 1 d R .
C34 C 1.3519(3) 0.3571(4) 0.8763(3) 0.0423(9) Uani 1 d . .
C35 C 1.2566(3) 0.2901(4) 0.8818(3) 0.0386(9) Uani 1 d . .
C36 C 1.1734(3) 0.3448(4) 0.9019(3) 0.0454(10) Uani 1 d . .
H36 H 1.1840(3) 0.4274(4) 0.9171(3) 0.080 Uiso 1 d R .
C37 C 1.0864(3) 0.2786(4) 0.9045(3) 0.0490(11) Uani 1 d . .
H37 H 1.0386(3) 0.3344(4) 0.9209(3) 0.080 Uiso 1 d R .
C38 C 1.1568(4) 0.1115(4) 0.8671(4) 0.0559(12) Uani 1 d . .
H38 H 1.1426(4) 0.0237(4) 0.8458(4) 0.080 Uiso 1 d R .
C39 C 1.2484(3) 0.1702(4) 0.8662(4) 0.0501(11) Uani 1 d . .
H39 H 1.3128 0.1361 0.8504 0.080 Uiso 1 d . .
Cl1 Cl 1.07076(9) -0.29409(9) 0.88872(7) 0.0436(3) Uani 1 d . .
O1 O 1.0446(3) -0.1928(3) 0.9328(3) 0.0676(10) Uani 1 d . .
O2 O 1.0365(4) -0.3961(3) 0.9262(3) 0.0876(13) Uani 1 d . .
O3 O 1.1825(3) -0.3021(5) 0.9127(5) 0.121(2) Uani 1 d . .
O4 O 1.0098(5) -0.2914(4) 0.7884(3) 0.095(2) Uani 1 d . .
O2W O 0.7500 0.1778(6) 0.2500 0.094(2) Uani 1 d S .
H2W H 0.6933 0.2211(6) 0.2122 0.080 Uiso 1 d R .
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'
Cl Cl 0.1484 0.1585 '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
N2 Zn1 N1 180.0 1_565 . ?
N2 Zn1 O1W 91.02(6) 1_565 2_656 ?
N1 Zn1 O1W 88.98(6) . 2_656 ?
N2 Zn1 O1W 91.02(6) 1_565 . ?
N1 Zn1 O1W 88.98(6) . . ?
O1W Zn1 O1W 177.97(12) 2_656 . ?
N2 Zn1 N3 91.71(7) 1_565 2_656 ?
N1 Zn1 N3 88.29(7) . 2_656 ?
O1W Zn1 N3 90.02(10) 2_656 2_656 ?
O1W Zn1 N3 89.92(10) . 2_656 ?
N2 Zn1 N3 91.71(7) 1_565 . ?
N1 Zn1 N3 88.29(7) . . ?
O1W Zn1 N3 89.92(10) 2_656 . ?
O1W Zn1 N3 90.02(10) . . ?
N3 Zn1 N3 176.58(14) 2_656 . ?
C11 N1 C11 115.9(4) . 2_656 ?
C11 N1 Zn1 122.1(2) . . ?
C11 N1 Zn1 122.1(2) 2_656 . ?
N1 C11 C12 124.0(3) . . ?
C11 C12 C13 118.9(3) . . ?
C12 C13 C12 118.2(4) . 2_656 ?
C12 C13 C14 120.9(2) . . ?
C12 C13 C14 120.9(2) 2_656 . ?
C15 C14 C15 118.1(4) 2_656 . ?
C15 C14 C13 120.9(2) 2_656 . ?
C15 C14 C13 120.9(2) . . ?
C16 C15 C14 119.1(3) . . ?
N2 C16 C15 123.8(3) . . ?
C16 N2 C16 116.1(4) . 2_656 ?
C16 N2 Zn1 122.0(2) . 1_545 ?
C16 N2 Zn1 122.0(2) 2_656 1_545 ?
C25 N3 C21 116.5(3) . . ?
C25 N3 Zn1 118.9(2) . . ?
C21 N3 Zn1 124.6(2) . . ?
Zn1 O1W N5 122.69(13) . . ?
Zn1 O1W O1 123.49(12) . . ?
N5 O1W O1 92.42(14) . . ?
N3 C21 C22 123.5(3) . . ?
C21 C22 C23 120.1(4) . . ?
C24 C23 C22 115.9(3) . . ?
C24 C23 C23 122.8(4) . 3_657 ?
C22 C23 C23 121.4(4) . 3_657 ?
C25 C24 C23 120.7(3) . . ?
N3 C25 C24 123.3(3) . . ?
C34 N4 C30 116.7(5) . . ?
C37 N5 C38 117.1(4) . . ?
C37 N5 O1W 128.2(3) . . ?
C38 N5 O1W 114.5(3) . . ?
N4 C30 C31 124.8(6) . . ?
C30 C31 C32 117.7(5) . . ?
C31 C32 C33 119.7(5) . . ?
C32 C33 C34 119.1(5) . . ?
N4 C34 C33 122.0(4) . . ?
N4 C34 C35 115.7(4) . . ?
C33 C34 C35 122.3(4) . . ?
C36 C35 C39 117.3(4) . . ?
C36 C35 C34 121.8(4) . . ?
C39 C35 C34 120.9(4) . . ?
C35 C36 C37 119.2(4) . . ?
N5 C37 C36 123.8(4) . . ?
N5 C38 C39 122.9(4) . . ?
C35 C39 C38 119.6(4) . . ?
O3 Cl1 O4 115.3(4) . . ?
O3 Cl1 O1 110.0(3) . . ?
O4 Cl1 O1 108.7(2) . . ?
O3 Cl1 O2 107.4(3) . . ?
O4 Cl1 O2 106.5(3) . . ?
O1 Cl1 O2 108.8(3) . . ?
Cl1 O1 O1W 138.5(2) . . ?
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
Zn1 N2 2.129(3) 1_565 ?
Zn1 N1 2.130(4) . ?
Zn1 O1W 2.189(3) 2_656 ?
Zn1 O1W 2.189(3) . ?
Zn1 N3 2.196(3) 2_656 ?
Zn1 N3 2.196(3) . ?
N1 C11 1.348(4) . ?
N1 C11 1.348(4) 2_656 ?
C11 C12 1.371(5) . ?
C12 C13 1.387(4) . ?
C13 C12 1.387(4) 2_656 ?
C13 C14 1.504(6) . ?
C14 C15 1.385(4) 2_656 ?
C14 C15 1.385(4) . ?
C15 C16 1.382(5) . ?
C16 N2 1.348(4) . ?
N2 C16 1.348(4) 2_656 ?
N2 Zn1 2.129(3) 1_545 ?
N3 C25 1.331(5) . ?
N3 C21 1.341(5) . ?
O1W N5 2.771(4) . ?
O1W O1 2.989(4) . ?
C21 C22 1.375(5) . ?
C22 C23 1.390(5) . ?
C23 C24 1.385(5) . ?
C23 C23 1.473(7) 3_657 ?
C24 C25 1.373(5) . ?
N4 C34 1.327(6) . ?
N4 C30 1.330(7) . ?
N5 C37 1.320(6) . ?
N5 C38 1.333(6) . ?
C30 C31 1.343(9) . ?
C31 C32 1.348(8) . ?
C32 C33 1.360(7) . ?
C33 C34 1.365(6) . ?
C34 C35 1.493(5) . ?
C35 C36 1.379(6) . ?
C35 C39 1.379(6) . ?
C36 C37 1.380(6) . ?
C38 C39 1.381(6) . ?
Cl1 O3 1.388(4) . ?
Cl1 O4 1.413(4) . ?
Cl1 O1 1.423(3) . ?
Cl1 O2 1.424(4) . ?
