#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/71/2227140.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_2227140
loop_
_publ_author_name
'Xie, Hong-Zhen'
'Zhang, Yan-Guang'
_publ_section_title
;
 μ-Adipato-bis[chlorido(2,2':6',2''-terpyridine)copper(II)]
 tetrahydrate
;
_journal_coeditor_code           ZL2287
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m934
_journal_paper_doi               10.1107/S1600536810027005
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu2 (C6 H8 O4) Cl2 (C15 H11 N3)2], 4H2 O'
_chemical_formula_moiety         'C36 H30 Cl2 Cu2 N6 O4, 4(H2 O)'
_chemical_formula_sum            'C36 H38 Cl2 Cu2 N6 O8'
_chemical_formula_weight         880.70
_chemical_name_systematic
;
μ-Adipato-bis[chlorido(2,2':6',2''-terpyridine)copper(II)] tetrahydrate
;
_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                83.42(3)
_cell_angle_beta                 81.69(3)
_cell_angle_gamma                84.38(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2334(16)
_cell_length_b                   9.5678(19)
_cell_length_c                   11.548(2)
_cell_measurement_reflns_used    7883
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.04
_cell_volume                     891.2(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '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  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8834
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        no
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.506
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0414P)²+0.4176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                3751
_reflns_number_total             4046
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2287.cif
_cod_data_source_block           I
_cod_database_code               2227140
_cod_database_fobs_code          2227140
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
Cu Cu 0.13815(3) 0.79530(2) 0.258347(18) 0.00798(8) Uani d . 1 . .
Cl Cl 0.00080(5) 0.61527(4) 0.17386(4) 0.01293(10) Uani d . 1 . .
O O1 0.31683(16) 0.65682(13) 0.29993(11) 0.0110(3) Uani d . 1 . .
O O2 0.41422(18) 0.84454(14) 0.35396(12) 0.0158(3) Uani d . 1 . .
O O3 0.40877(18) 0.42538(14) 0.16550(12) 0.0173(3) Uani d . 1 . .
H H3C 0.5094 0.4458 0.1431 0.021 Uiso d . 1 . .
H H3D 0.3784 0.4760 0.2132 0.021 Uiso d . 1 . .
O O4 -0.30631(19) 0.54262(18) 0.05804(13) 0.0244(3) Uani d . 1 . .
H H4C -0.2000 0.5478 0.0749 0.029 Uiso d . 1 . .
H H4D -0.2994 0.5637 -0.0183 0.029 Uiso d . 1 . .
N N1 -0.00477(19) 0.78588(16) 0.41703(13) 0.0093(3) Uani d . 1 . .
N N2 0.01050(18) 0.97845(15) 0.24509(13) 0.0089(3) Uani d . 1 . .
N N3 0.24603(19) 0.88021(16) 0.10055(13) 0.0097(3) Uani d . 1 . .
C C1 -0.0037(2) 0.67745(19) 0.50071(16) 0.0121(3) Uani d . 1 . .
H H1A 0.0753 0.6020 0.4902 0.014 Uiso calc R 1 . .
C C2 -0.1158(2) 0.6730(2) 0.60277(16) 0.0139(4) Uani d . 1 . .
H H2A -0.1120 0.5962 0.6598 0.017 Uiso calc R 1 . .
C C3 -0.2338(2) 0.7858(2) 0.61759(16) 0.0151(4) Uani d . 1 . .
H H3A -0.3115 0.7851 0.6846 0.018 Uiso calc R 1 . .
C C4 -0.2350(2) 0.90009(19) 0.53138(16) 0.0131(4) Uani d . 1 . .
H H4A -0.3123 0.9771 0.5404 0.016 Uiso calc R 1 . .
C C5 -0.1188(2) 0.89694(18) 0.43166(16) 0.0098(3) Uani d . 1 . .
C C6 -0.1046(2) 1.01126(19) 0.33414(16) 0.0104(3) Uani d . 1 . .
C C7 -0.1938(2) 1.14257(19) 0.33008(16) 0.0128(4) Uani d . 1 . .
H H7A -0.2752 1.1655 0.3912 0.015 Uiso calc R 1 . .
C C8 -0.1577(2) 1.23842(19) 0.23184(17) 0.0138(4) Uani d . 1 . .
H H8A -0.2157 1.3269 0.2272 0.017 Uiso calc R 1 . .
C C9 -0.0360(2) 1.20397(19) 0.14023(16) 0.0126(4) Uani d . 1 . .
H H9A -0.0112 1.2683 0.0748 0.015 Uiso calc R 1 . .
C C10 0.0474(2) 1.06991(18) 0.14981(16) 0.0100(3) Uani d . 1 . .
C C11 0.1807(2) 1.01092(18) 0.06390(15) 0.0093(3) Uani d . 1 . .
C C12 0.2341(2) 1.07967(19) -0.04513(16) 0.0122(3) Uani d . 1 . .
H H12A 0.1876 1.1691 -0.0687 0.015 Uiso calc R 1 . .
C C13 0.3592(2) 1.0118(2) -0.11900(16) 0.0134(4) Uani d . 1 . .
H H13A 0.3983 1.0557 -0.1924 0.016 Uiso calc R 1 . .
C C14 0.4240(2) 0.8782(2) -0.08133(16) 0.0137(4) Uani d . 1 . .
H H14A 0.5065 0.8308 -0.1296 0.016 Uiso calc R 1 . .
C C15 0.3649(2) 0.81548(19) 0.02906(16) 0.0117(3) Uani d . 1 . .
H H15A 0.4092 0.7258 0.0541 0.014 Uiso calc R 1 . .
C C16 0.4287(2) 0.71750(18) 0.33897(15) 0.0095(3) Uani d . 1 . .
C C17 0.5825(2) 0.62512(19) 0.36324(16) 0.0121(3) Uani d . 1 . .
H H17A 0.6498 0.6774 0.4025 0.015 Uiso calc R 1 . .
H H17B 0.6456 0.6031 0.2890 0.015 Uiso calc R 1 . .
C C18 0.5460(2) 0.48718(19) 0.43937(15) 0.0117(4) Uani d . 1 . .
H H18A 0.4804 0.4338 0.3997 0.014 Uiso calc R 1 . .
H H18C 0.6489 0.4311 0.4487 0.014 Uiso calc R 1 . .
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'
Cl Cl 0.1484 0.1585 '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_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Cu O1 . . 157.68(6) ?
N2 Cu N3 . . 79.61(7) ?
O1 Cu N3 . . 99.40(6) ?
N2 Cu N1 . . 79.49(7) ?
O1 Cu N1 . . 98.23(6) ?
N3 Cu N1 . . 158.62(6) ?
N2 Cu Cl . . 110.17(5) ?
O1 Cu Cl . . 92.15(4) ?
N3 Cu Cl . . 94.79(5) ?
N1 Cu Cl . . 96.54(5) ?
C16 O1 Cu . . 110.59(11) ?
H3C O3 H3D . . 102.7 ?
H4C O4 H4D . . 104.5 ?
C1 N1 C5 . . 119.25(16) ?
C1 N1 Cu . . 125.82(13) ?
C5 N1 Cu . . 114.70(12) ?
C6 N2 C10 . . 122.21(15) ?
C6 N2 Cu . . 118.81(12) ?
C10 N2 Cu . . 118.88(12) ?
C15 N3 C11 . . 119.08(16) ?
C15 N3 Cu . . 125.77(12) ?
C11 N3 Cu . . 114.98(12) ?
N1 C1 C2 . . 122.57(17) ?
N1 C1 H1A . . 118.7 ?
C2 C1 H1A . . 118.7 ?
C1 C2 C3 . . 118.37(18) ?
C1 C2 H2A . . 120.8 ?
C3 C2 H2A . . 120.8 ?
C2 C3 C4 . . 119.53(18) ?
C2 C3 H3A . . 120.2 ?
C4 C3 H3A . . 120.2 ?
C5 C4 C3 . . 118.75(17) ?
C5 C4 H4A . . 120.6 ?
C3 C4 H4A . . 120.6 ?
N1 C5 C4 . . 121.52(17) ?
N1 C5 C6 . . 113.96(16) ?
C4 C5 C6 . . 124.51(16) ?
N2 C6 C7 . . 120.59(17) ?
N2 C6 C5 . . 112.72(15) ?
C7 C6 C5 . . 126.68(17) ?
C8 C7 C6 . . 117.98(17) ?
C8 C7 H7A . . 121.0 ?
C6 C7 H7A . . 121.0 ?
C7 C8 C9 . . 121.01(17) ?
C7 C8 H8A . . 119.5 ?
C9 C8 H8A . . 119.5 ?
C8 C9 C10 . . 117.87(17) ?
C8 C9 H9A . . 121.1 ?
C10 C9 H9A . . 121.1 ?
N2 C10 C9 . . 120.32(17) ?
N2 C10 C11 . . 112.50(15) ?
C9 C10 C11 . . 127.18(17) ?
N3 C11 C12 . . 122.00(16) ?
N3 C11 C10 . . 113.92(15) ?
C12 C11 C10 . . 124.06(16) ?
C11 C12 C13 . . 118.57(17) ?
C11 C12 H12A . . 120.7 ?
C13 C12 H12A . . 120.7 ?
C14 C13 C12 . . 119.01(17) ?
C14 C13 H13A . . 120.5 ?
C12 C13 H13A . . 120.5 ?
C13 C14 C15 . . 119.40(17) ?
C13 C14 H14A . . 120.3 ?
C15 C14 H14A . . 120.3 ?
N3 C15 C14 . . 121.92(17) ?
N3 C15 H15A . . 119.0 ?
C14 C15 H15A . . 119.0 ?
O2 C16 O1 . . 122.70(17) ?
O2 C16 C17 . . 121.07(17) ?
O1 C16 C17 . . 116.22(15) ?
C16 C17 C18 . . 113.19(15) ?
C16 C17 H17A . . 108.9 ?
C18 C17 H17A . . 108.9 ?
C16 C17 H17B . . 108.9 ?
C18 C17 H17B . . 108.9 ?
H17A C17 H17B . . 107.8 ?
C18 C18 C17 2_666 . 112.17(18) ?
C18 C18 H18A 2_666 . 109.2 ?
C17 C18 H18A . . 109.2 ?
C18 C18 H18C 2_666 . 109.2 ?
C17 C18 H18C . . 109.2 ?
H18A C18 H18C . . 107.9 ?
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
Cu N2 . 1.9552(16) ?
Cu O1 . 1.9562(14) ?
Cu N3 . 2.0257(17) ?
Cu N1 . 2.0274(16) ?
Cu Cl . 2.5067(8) ?
O1 C16 . 1.294(2) ?
O2 C16 . 1.239(2) ?
O3 H3C . 0.8658 ?
O3 H3D . 0.7734 ?
O4 H4C . 0.9308 ?
O4 H4D . 0.8764 ?
N1 C1 . 1.335(2) ?
N1 C5 . 1.356(2) ?
N2 C6 . 1.337(2) ?
N2 C10 . 1.343(2) ?
N3 C15 . 1.337(2) ?
N3 C11 . 1.358(2) ?
C1 C2 . 1.387(3) ?
C1 H1A . 0.9300 ?
C2 C3 . 1.389(3) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.392(3) ?
C3 H3A . 0.9300 ?
C4 C5 . 1.388(3) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.478(3) ?
C6 C7 . 1.391(2) ?
C7 C8 . 1.391(3) ?
C7 H7A . 0.9300 ?
C8 C9 . 1.393(3) ?
C8 H8A . 0.9300 ?
C9 C10 . 1.395(2) ?
C9 H9A . 0.9300 ?
C10 C11 . 1.483(2) ?
C11 C12 . 1.385(3) ?
C12 C13 . 1.397(3) ?
C12 H12A . 0.9300 ?
C13 C14 . 1.383(3) ?
C13 H13A . 0.9300 ?
C14 C15 . 1.387(3) ?
C14 H14A . 0.9300 ?
C15 H15A . 0.9300 ?
C16 C17 . 1.513(3) ?
C17 C18 . 1.530(3) ?
C17 H17A . 0.9700 ?
C17 H17B . 0.9700 ?
C18 C18 2_666 1.527(3) ?
C18 H18A . 0.9700 ?
C18 H18C . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O3 H3C O4 1_655 0.87 1.94 2.767(2) 160 yes
O3 H3D O1 ? 0.77 2.08 2.829(2) 163 yes
O4 H4C Cl ? 0.93 2.32 3.194(2) 156 yes
O4 H4D O3 2_565 0.88 2.02 2.805(2) 148 yes
