#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179379 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/76/4327647.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_4327647
loop_
_publ_author_name
'Ming-Liang Tong'
'Hong-Ji Chen'
'Xiao-Ming Chen'
_publ_contact_author
;
      Chen, Xiao-Ming
      School of Chemistry and Chemical Engineering
      Zhongshan University
      Guangzhou, 510275
      P. R. China
;
_publ_contact_author_email       cescxm@zsu.edu.cn
_publ_contact_author_fax         '86 20 84112245'
_publ_contact_author_phone       86-20-84112074
_publ_section_title
;
 Molecular Ladders with Multiple Interpenetration of the Lateral Arms into
 the Squares of Adjacent Ladders Observed for
 [M2(4,4'-bpy)3(H2O)2(phba)2](NO3)2.4H2O (M = Cu2+ or Co2+; 4,4'-bpy =
 4,4'-Bipyridine; phba = 4-Hydroxybenzoate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2235
_journal_page_last               2238
_journal_paper_doi               10.1021/ic991312+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C44 H46 Cu2 N8 O18'
_chemical_formula_weight         1101.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.02
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.023(3)
_cell_length_b                   15.398(8)
_cell_length_c                   14.315(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     2335.4(19)
_computing_cell_refinement       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_collection       'SHELXTL-Plus (Sheldrick, 1990)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL-97, V.5.0 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Siemens R3m'
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5341
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep blue'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0000(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          1.001
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0595P)²+1.7031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                3782
_reflns_number_total             5085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9913122B_2.cif
_cod_data_source_block           complex1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+1.7031P] 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^)+(0.0595P)^2^+1.7031P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4327647
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.14247(3) 0.16817(2) 0.14087(3) 0.02449(12) Uani 1 d .
N1 N 0.3254(2) 0.16933(16) 0.14284(18) 0.0260(5) Uani 1 d .
N2 N 0.9633(2) 0.16155(16) 0.14646(18) 0.0281(5) Uani 1 d .
N3 N 0.1050(2) 0.29113(16) 0.08745(19) 0.0296(6) Uani 1 d .
O1 O 0.17880(19) 0.06489(13) 0.22800(15) 0.0292(5) Uani 1 d .
O2 O 0.2128(2) 0.18088(14) 0.31948(17) 0.0402(6) Uani 1 d .
O3 O 0.4146(4) -0.1025(2) 0.6397(2) 0.0997(15) Uani 1 d .
H3 H 0.4288 -0.1418 0.6295 0.050 Uiso 1 d R
C1 C 0.3977(3) 0.2400(2) 0.1574(2) 0.0330(7) Uani 1 d .
H1A H 0.3604 0.2942 0.1675 0.080 Uiso 1 d R
C2 C 0.5220(3) 0.2390(2) 0.1591(3) 0.0335(7) Uani 1 d .
H2A H 0.5702 0.2918 0.1691 0.080 Uiso 1 d R
C3 C 0.5782(3) 0.1616(2) 0.1468(2) 0.0276(6) Uani 1 d .
C4 C 0.5039(3) 0.0878(2) 0.1327(2) 0.0316(7) Uani 1 d .
H4A H 0.5394 0.0325 0.1239 0.080 Uiso 1 d R
C5 C 0.37959(19) 0.09410(14) 0.13131(17) 0.0307(7) Uani 1 d .
H5A H 0.3294 0.0422 0.1219 0.080 Uiso 1 d R
C6 C 0.88395(19) 0.10077(14) 0.09839(17) 0.0337(7) Uani 1 d R
H6A H 0.9151 0.0578 0.0622 0.080 Uiso 1 d R
C7 C 0.7596(3) 0.0969(2) 0.0986(3) 0.0351(7) Uani 1 d .
H7A H 0.7059 0.0519 0.0633 0.080 Uiso 1 d R
C8 C 0.7122(3) 0.15838(19) 0.1496(2) 0.0269(6) Uani 1 d .
C9 C 0.7963(3) 0.2190(2) 0.2017(2) 0.0333(7) Uani 1 d .
H9A H 0.7687 0.2615 0.2404 0.080 Uiso 1 d R
C10 C 0.9184(3) 0.2187(2) 0.1984(2) 0.0348(7) Uani 1 d .
H10A H 0.9748 0.2616 0.2353 0.080 Uiso 1 d R
C11 C 0.0422(4) 0.3042(2) -0.0044(3) 0.0433(8) Uani 1 d .
H11A H 0.0248 0.2551 -0.0474 0.080 Uiso 1 d R
C12 C 0.0006(4) 0.3842(2) -0.0408(3) 0.0461(9) Uani 1 d .
H12A H -0.0443 0.3905 -0.1082 0.080 Uiso 1 d R
C13 C 0.0224(3) 0.45618(19) 0.0185(2) 0.0299(7) Uani 1 d .
C14 C 0.0893(3) 0.4424(2) 0.1138(2) 0.0385(8) Uani 1 d .
H14A H 0.1087 0.4904 0.1582 0.080 Uiso 1 d R
C15 C 0.1277(3) 0.3603(2) 0.1449(2) 0.0368(7) Uani 1 d .
H15A H 0.1737 0.3522 0.2118 0.080 Uiso 1 d R
C16 C 0.2175(3) 0.1009(2) 0.3115(2) 0.0296(7) Uani 1 d .
C17 C 0.2693(3) 0.0453(2) 0.3965(2) 0.0310(7) Uani 1 d .
C18 C 0.3367(3) 0.0819(2) 0.4836(2) 0.0407(8) Uani 1 d .
H18A H 0.3505 0.1435 0.4877 0.080 Uiso 1 d R
C19 C 0.3849(4) 0.0312(2) 0.5641(3) 0.0499(10) Uani 1 d .
H19A H 0.4319 0.0571 0.6242 0.080 Uiso 1 d R
C20 C 0.3664(4) -0.0568(3) 0.5587(3) 0.0551(11) Uani 1 d .
C21 C 0.2992(4) -0.0944(2) 0.4728(3) 0.0467(9) Uani 1 d .
H21A H 0.2855 -0.1560 0.4694 0.080 Uiso 1 d R
C22 C 0.2514(3) -0.0434(2) 0.3924(2) 0.0379(8) Uani 1 d .
H22A H 0.2051 -0.0699 0.3324 0.080 Uiso 1 d R
O1W O 0.1097(2) 0.10048(14) -0.00499(16) 0.0368(5) Uani 1 d .
H1WA H 0.1647 0.1138 -0.0304 0.050 Uiso 1 d R
H1WB H 0.0428 0.0957 -0.0368 0.050 Uiso 1 d R
O3W O 0.2756(3) 0.34314(18) 0.3942(2) 0.0596(8) Uani 1 d .
H3WA H 0.2627 0.2916 0.3911 0.050 Uiso 1 d R
H3WB H 0.3390 0.3469 0.4043 0.050 Uiso 1 d R
O2W O 0.1111(2) -0.09808(17) 0.14511(18) 0.0514(7) Uani 1 d .
H2WA H 0.1682 -0.1185 0.1370 0.050 Uiso 1 d R
H2WB H 0.1348 -0.0543 0.1680 0.050 Uiso 1 d R
N4 N 0.3978(4) -0.1793(2) 0.1109(3) 0.0604(9) Uani 1 d .
O4 O 0.2968(3) -0.2120(2) 0.1115(3) 0.0761(9) Uani 1 d .
O5 O 0.4727(3) -0.2253(3) 0.0862(3) 0.0941(12) Uani 1 d .
O6 O 0.4203(5) -0.1065(2) 0.1332(5) 0.155(2) Uani 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'
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'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 N2 87.96(9) . 1_455
O1 Cu1 N1 88.32(9) . .
N2 Cu1 N1 176.17(10) 1_455 .
O1 Cu1 N3 163.73(10) . .
N2 Cu1 N3 87.85(10) 1_455 .
N1 Cu1 N3 95.47(10) . .
O1 Cu1 O1W 99.36(9) . .
N2 Cu1 O1W 96.03(9) 1_455 .
N1 Cu1 O1W 85.49(9) . .
N3 Cu1 O1W 96.71(10) . .
O1 Cu1 O2 57.52(8) . .
N2 Cu1 O2 89.65(9) 1_455 .
N1 Cu1 O2 87.58(9) . .
N3 Cu1 O2 106.74(9) . .
O1W Cu1 O2 156.08(8) . .
C1 N1 C5 117.4(2) . .
C1 N1 Cu1 124.4(2) . .
C5 N1 Cu1 118.20(17) . .
C10 N2 C6 117.3(2) . .
C10 N2 Cu1 120.8(2) . 1_655
C6 N2 Cu1 121.91(18) . 1_655
C11 N3 C15 116.8(3) . .
C11 N3 Cu1 120.7(2) . .
C15 N3 Cu1 121.9(2) . .
C16 O1 Cu1 101.34(18) . .
C16 O1 O2W 140.23(19) . .
Cu1 O1 O2W 117.91(11) . .
C16 O2 Cu1 80.47(19) . .
C16 O2 O3W 158.9(2) . .
Cu1 O2 O3W 116.87(11) . .
C20 O3 O5 108.5(3) . 4_556
N1 C1 C2 123.3(3) . .
C1 C2 C3 119.5(3) . .
C2 C3 C4 117.4(3) . .
C2 C3 C8 120.7(3) . .
C4 C3 C8 121.9(3) . .
C5 C4 C3 119.7(3) . .
N1 C5 C4 122.7(2) . .
N2 C6 C7 122.8(2) . .
C6 C7 C8 119.6(3) . .
C9 C8 C7 116.9(3) . .
C9 C8 C3 120.9(3) . .
C7 C8 C3 122.2(3) . .
C10 C9 C8 120.2(3) . .
N2 C10 C9 123.0(3) . .
N3 C11 C12 123.1(3) . .
C11 C12 C13 120.5(3) . .
C12 C13 C14 116.3(3) . .
C12 C13 C13 121.8(4) . 3_565
C14 C13 C13 121.9(4) . 3_565
C15 C14 C13 119.8(3) . .
N3 C15 C14 123.5(3) . .
O2 C16 O1 120.4(3) . .
O2 C16 C17 121.3(3) . .
O1 C16 C17 118.4(3) . .
C22 C17 C18 118.4(3) . .
C22 C17 C16 121.6(3) . .
C18 C17 C16 120.0(3) . .
C19 C18 C17 120.9(3) . .
C20 C19 C18 119.8(3) . .
O3 C20 C19 117.0(4) . .
O3 C20 C21 122.8(4) . .
C19 C20 C21 120.1(3) . .
C22 C21 C20 119.8(3) . .
C21 C22 C17 120.9(3) . .
Cu1 O1W O2W 124.92(11) . 3
Cu1 O1W O3W 112.05(11) . 4_565
O2W O1W O3W 102.00(12) 3 4_565
O2 O3W O5 80.69(12) . 2_655
O1 O2W O4 120.54(12) . .
O6 N4 O5 121.9(5) . .
O6 N4 O4 121.0(5) . .
O5 N4 O4 117.1(4) . .
N4 O4 O2W 116.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.992(2) .
Cu1 N2 2.001(2) 1_455
Cu1 N1 2.009(2) .
Cu1 N3 2.041(3) .
Cu1 O1W 2.272(2) .
Cu1 O2 2.466(3) .
N1 C1 1.330(4) .
N1 C5 1.334(3) .
N2 C10 1.332(4) .
N2 C6 1.335(3) .
N2 Cu1 2.001(2) 1_655
N3 C11 1.322(4) .
N3 C15 1.327(4) .
O1 C16 1.279(4) .
O1 O2W 2.788(3) .
O2 C16 1.240(4) .
O2 O3W 2.731(4) .
O3 C20 1.335(4) .
O3 O5 2.881(6) 4_556
C1 C2 1.364(4) .
C2 C3 1.376(4) .
C3 C4 1.382(4) .
C3 C8 1.467(4) .
C4 C5 1.368(3) .
C6 C7 1.373(4) .
C7 C8 1.383(4) .
C8 C9 1.380(4) .
C9 C10 1.360(4) .
C11 C12 1.367(5) .
C12 C13 1.376(5) .
C13 C14 1.376(4) .
C13 C13 1.484(6) 3_565
C14 C15 1.368(4) .
C16 C17 1.468(4) .
C17 C22 1.380(4) .
C17 C18 1.383(5) .
C18 C19 1.372(5) .
C19 C20 1.369(5) .
C20 C21 1.376(5) .
C21 C22 1.372(5) .
O1W O2W 2.694(3) 3
O1W O3W 2.763(4) 4_565
O3W O5 2.908(5) 2_655
O2W O4 2.836(4) .
N4 O6 1.174(5) .
N4 O5 1.212(5) .
N4 O4 1.224(5) .
