#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/43/2204321.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_2204321
loop_
_publ_author_name
'Hong-Ping Xiao'
'Qian Shi'
'Ming-De Ye'
_publ_section_title
;
 Di-μ-5-hydroxyisophthalato-bis[aqua(1,10-phenanthroline)copper(II)]
 trihydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1498
_journal_page_last               m1500
_journal_paper_doi               10.1107/S1600536804023190
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'[Cu2 (C8 H4 O5)2 (C12 H8 N2)2 (H2 O)2], 3H2 O'
_chemical_formula_moiety         'C40 H28 Cu2 N4 O12, 3H2 O'
_chemical_formula_sum            'C40 H34 Cu2 N4 O15'
_chemical_formula_weight         937.79
_chemical_name_systematic
;Di-μ-5-hydroxyisophthalato-bis[aqua(1,10-phenanthroline)copper(II)]
 trihydrate
;
_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                97.482(2)
_cell_angle_beta                 92.284(2)
_cell_angle_gamma                101.475(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2751(10)
_cell_length_b                   10.4797(14)
_cell_length_c                   12.7575(17)
_cell_measurement_reflns_used    1209
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.33
_cell_measurement_theta_min      2.89
_cell_volume                     942.9(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Bruker, 2002)'
_computing_publication_material  'SHELXTL (Bruker, 2002)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6956
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  0.8886
_exptl_absorpt_correction_T_min  0.7519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.336
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3383
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0838
_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)+(0.0361P)²+4.7073P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                3353
_reflns_number_total             3383
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv6376.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2204321
_cod_database_fobs_code          2204321
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_type_symbol
Cu1 0.56165(10) 0.94671(7) 0.77592(6) 0.0210(2) Uani d . 1 Cu
O1 0.8321(6) 1.0023(5) 0.6939(4) 0.0343(11) Uani d . 1 O
O2 1.1211(6) 1.1180(4) 0.7375(4) 0.0398(12) Uani d . 1 O
O3 1.3257(7) 0.9752(4) 1.0839(3) 0.0317(11) Uani d . 1 O
O4 1.3084(7) 0.7613(4) 1.0883(4) 0.0372(12) Uani d . 1 O
O5 0.9753(7) 0.5502(4) 0.7323(4) 0.0371(12) Uani d . 1 O
H5 1.0170 0.4982 0.7647 0.056 Uiso calc R 1 H
O6 0.4817(6) 1.1077(4) 0.7444(3) 0.0286(10) Uani d D 1 O
H6B 0.3674 1.0981 0.7473 0.043 Uiso calc R 1 H
H6C 0.5343 1.1533 0.7984 0.043 Uiso d RD 1 H
O8 0.7893(16) 0.8366(9) 0.4906(7) 0.040(2) Uani d PD 0.50 O
N1 0.5685(7) 0.7675(5) 0.8149(4) 0.0243(11) Uani d . 1 N
N2 0.4239(7) 0.8399(5) 0.6453(4) 0.0244(11) Uani d . 1 N
C1 0.6418(9) 0.7354(7) 0.9015(5) 0.0326(15) Uani d . 1 C
H1 0.6987 0.8021 0.9551 0.039 Uiso calc R 1 H
C2 0.6371(10) 0.6045(7) 0.9156(6) 0.0381(17) Uani d . 1 C
H2 0.6893 0.5847 0.9776 0.046 Uiso calc R 1 H
C3 0.5555(11) 0.5075(7) 0.8375(6) 0.0431(18) Uani d . 1 C
H3 0.5527 0.4204 0.8461 0.052 Uiso calc R 1 H
C4 0.4753(9) 0.5360(6) 0.7443(6) 0.0340(16) Uani d . 1 C
C5 0.3827(11) 0.4412(7) 0.6579(6) 0.0441(19) Uani d . 1 C
H5A 0.3749 0.3521 0.6611 0.053 Uiso calc R 1 H
C6 0.3073(11) 0.4786(7) 0.5726(6) 0.0428(18) Uani d . 1 C
H6A 0.2465 0.4146 0.5181 0.051 Uiso calc R 1 H
C7 0.3173(9) 0.6146(7) 0.5627(5) 0.0332(15) Uani d . 1 C
C8 0.2417(11) 0.6603(8) 0.4761(6) 0.0444(19) Uani d . 1 C
H8 0.1790 0.6010 0.4192 0.053 Uiso calc R 1 H
C9 0.2599(10) 0.7912(8) 0.4750(5) 0.0410(18) Uani d . 1 C
H9 0.2115 0.8223 0.4170 0.049 Uiso calc R 1 H
C10 0.3515(9) 0.8789(7) 0.5615(5) 0.0333(15) Uani d . 1 C
H10 0.3621 0.9686 0.5601 0.040 Uiso calc R 1 H
C11 0.4084(9) 0.7087(6) 0.6452(5) 0.0267(14) Uani d . 1 C
C12 0.4873(8) 0.6696(6) 0.7367(5) 0.0234(13) Uani d . 1 C
C13 0.9937(9) 1.0161(6) 0.7352(5) 0.0279(14) Uani d . 1 C
C14 1.0433(8) 0.9042(6) 0.7871(5) 0.0229(13) Uani d . 1 C
C15 1.1397(9) 0.9297(6) 0.8854(5) 0.0251(13) Uani d . 1 C
H15 1.1789 1.0161 0.9182 0.030 Uiso calc R 1 H
C16 1.1785(8) 0.8275(6) 0.9358(5) 0.0223(12) Uani d . 1 C
C17 1.2784(9) 0.8555(6) 1.0440(5) 0.0251(13) Uani d . 1 C
C18 1.1244(8) 0.6993(6) 0.8857(5) 0.0248(13) Uani d . 1 C
H18 1.1510 0.6305 0.9189 0.030 Uiso calc R 1 H
C19 1.0301(9) 0.6734(6) 0.7859(5) 0.0258(13) Uani d . 1 C
C20 0.9855(9) 0.7759(6) 0.7379(5) 0.0259(13) Uani d . 1 C
H20 0.9168 0.7583 0.6728 0.031 Uiso calc R 1 H
H8B 0.847(18) 0.852(12) 0.440(6) 0.039 Uiso d PD 0.50 H
H8C 0.794(19) 0.889(9) 0.541(6) 0.039 Uiso d PD 0.50 H
O7 0.0422(9) 0.3563(5) 0.8358(5) 0.0556(16) Uani d D 1 O
H7B 0.062(10) 0.293(5) 0.799(5) 0.03(2) Uiso d D 1 H
H7C -0.060(6) 0.331(7) 0.858(6) 0.04(2) Uiso d D 1 H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Cu1 O6 2_777 . 94.36(18) yes
O3 Cu1 N2 2_777 . 169.7(2) yes
O6 Cu1 N2 . . 92.6(2) yes
O3 Cu1 N1 2_777 . 89.20(19) yes
O6 Cu1 N1 . . 164.33(19) yes
N2 Cu1 N1 . . 82.1(2) yes
O3 Cu1 O1 2_777 . 94.25(19) yes
O6 Cu1 O1 . . 90.84(18) yes
N2 Cu1 O1 . . 93.33(19) yes
N1 Cu1 O1 . . 104.13(18) yes
C13 O1 Cu1 . . 125.5(4) ?
C17 O3 Cu1 . 2_777 129.8(4) ?
C19 O5 H5 . . 109.5 ?
Cu1 O6 H6B . . 109.5 ?
Cu1 O6 H6C . . 94.6 ?
H6B O6 H6C . . 109.6 ?
H8B O8 H8C . . 122(6) ?
C1 N1 C12 . . 118.4(6) ?
C1 N1 Cu1 . . 129.5(5) ?
C12 N1 Cu1 . . 112.1(4) ?
C10 N2 C11 . . 117.7(5) ?
C10 N2 Cu1 . . 129.4(4) ?
C11 N2 Cu1 . . 112.9(4) ?
N1 C1 C2 . . 122.3(7) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C3 C2 C1 . . 119.0(7) ?
C3 C2 H2 . . 120.5 ?
C1 C2 H2 . . 120.5 ?
C2 C3 C4 . . 121.1(7) ?
C2 C3 H3 . . 119.5 ?
C4 C3 H3 . . 119.5 ?
C3 C4 C12 . . 116.1(7) ?
C3 C4 C5 . . 125.6(7) ?
C12 C4 C5 . . 118.3(7) ?
C6 C5 C4 . . 121.0(7) ?
C6 C5 H5A . . 119.5 ?
C4 C5 H5A . . 119.5 ?
C5 C6 C7 . . 121.9(7) ?
C5 C6 H6A . . 119.0 ?
C7 C6 H6A . . 119.0 ?
C11 C7 C8 . . 117.0(6) ?
C11 C7 C6 . . 118.1(6) ?
C8 C7 C6 . . 124.9(7) ?
C9 C8 C7 . . 119.9(7) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C8 C9 C10 . . 119.5(7) ?
C8 C9 H9 . . 120.3 ?
C10 C9 H9 . . 120.3 ?
N2 C10 C9 . . 122.6(6) ?
N2 C10 H10 . . 118.7 ?
C9 C10 H10 . . 118.7 ?
N2 C11 C7 . . 123.3(6) ?
N2 C11 C12 . . 116.4(5) ?
C7 C11 C12 . . 120.3(6) ?
N1 C12 C4 . . 123.1(6) ?
N1 C12 C11 . . 116.5(5) ?
C4 C12 C11 . . 120.3(6) ?
O1 C13 O2 . . 124.5(6) ?
O1 C13 C14 . . 118.4(6) ?
O2 C13 C14 . . 117.0(5) ?
C15 C14 C20 . . 119.9(6) ?
C15 C14 C13 . . 120.1(5) ?
C20 C14 C13 . . 120.0(6) ?
C14 C15 C16 . . 120.6(6) ?
C14 C15 H15 . . 119.7 ?
C16 C15 H15 . . 119.7 ?
C18 C16 C15 . . 119.6(6) ?
C18 C16 C17 . . 120.0(5) ?
C15 C16 C17 . . 120.3(5) ?
O4 C17 O3 . . 124.8(6) ?
O4 C17 C16 . . 118.9(5) ?
O3 C17 C16 . . 116.3(5) ?
C16 C18 C19 . . 120.0(6) ?
C16 C18 H18 . . 120.0 ?
C19 C18 H18 . . 120.0 ?
O5 C19 C20 . . 117.3(6) ?
O5 C19 C18 . . 122.8(6) ?
C20 C19 C18 . . 119.9(6) ?
C14 C20 C19 . . 120.0(6) ?
C14 C20 H20 . . 120.0 ?
C19 C20 H20 . . 120.0 ?
H7B O7 H7C . . 104(8) ?
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
Cu1 O3 2_777 1.942(4) yes
Cu1 O6 . 1.974(4) yes
Cu1 N2 . 1.992(5) yes
Cu1 N1 . 2.013(5) yes
Cu1 O1 . 2.274(5) yes
O1 C13 . 1.243(8) ?
O2 C13 . 1.263(8) ?
O3 C17 . 1.265(7) ?
O3 Cu1 2_777 1.942(4) ?
O4 C17 . 1.250(7) ?
O5 C19 . 1.355(7) ?
O5 H5 . 0.8200 ?
O6 H6B . 0.8200 ?
O6 H6C . 0.8185 ?
O8 H8B . 0.80(3) ?
O8 H8C . 0.79(3) ?
N1 C1 . 1.319(8) ?
N1 C12 . 1.356(8) ?
N2 C10 . 1.321(8) ?
N2 C11 . 1.357(8) ?
C1 C2 . 1.400(9) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.351(11) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.397(11) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.402(9) ?
C4 C5 . 1.430(10) ?
C5 C6 . 1.337(11) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.434(10) ?
C6 H6A . 0.9300 ?
C7 C11 . 1.391(9) ?
C7 C8 . 1.396(10) ?
C8 C9 . 1.353(11) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.393(9) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.423(9) ?
C13 C14 . 1.515(9) ?
C14 C15 . 1.380(8) ?
C14 C20 . 1.383(8) ?
C15 C16 . 1.387(8) ?
C15 H15 . 0.9300 ?
C16 C18 . 1.384(8) ?
C16 C17 . 1.500(8) ?
C18 C19 . 1.390(9) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.389(9) ?
C20 H20 . 0.9300 ?
O7 H7B . 0.81(3) ?
O7 H7C . 0.81(3) ?
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
O5 H5 O7 1_655 0.82 1.88 2.673(8) 164
O6 H6B O2 1_455 0.82 1.85 2.645(6) 164
O6 H6C O4 2_777 0.82 1.82 2.630(6) 168
O6 H6C O3 2_777 0.82 2.46 2.872(6) 112
O8 H8B O2 2_776 0.80(3) 2.35(7) 3.084(11) 155(14)
O8 H8C O1 . 0.79(3) 2.12(4) 2.896(10) 168(15)
O7 H7B O2 1_445 0.81(3) 2.03(3) 2.820(8) 167(8)
O7 H7C O4 2_667 0.81(3) 2.06(3) 2.867(8) 171(7)
