#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/32/2203281.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_2203281
loop_
_publ_author_name
'Yang, Hong-Fang'
'Huang, Chang-Cang'
'Zhang, Han-Hui'
'Liu, Yongxiu'
'Lian, Zhao-Xun'
Xiao,Guang-Can
_publ_section_title
;
 A new mixed-valence CuII/CuI complex:
 chlorobis(1,10-phenanthroline)copper(II) dichlorocuprate(I)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m291
_journal_page_last               m293
_journal_paper_doi               10.1107/S1600536804002375
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Cu Cl (C12 H8 N2)2] [Cu Cl2]'
_chemical_formula_moiety         'C24 H16 Cl Cu N4 1+, Cl2 Cu 1-'
_chemical_formula_sum            'C24 H16 Cl3 Cu2 N4'
_chemical_formula_weight         593.86
_chemical_name_systematic
;
chlorobis(1,10-phenanthroline)copper(II) dichlorocuprate(I)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 111.480(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4063(5)
_cell_length_b                   12.6196(6)
_cell_length_c                   13.3400(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2256.79(16)
_computing_cell_refinement       TEXRAY
_computing_data_collection
'TEXRAY (Molecular Structure Corporation, 1999)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Weissenberg IP'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotor target'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5081
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.261
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.435
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0351
_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)+(0.0676P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                3786
_reflns_number_total             5081
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv6258.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2203281
_cod_database_fobs_code          2203281
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
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 0.25883(2) 0.22733(3) 0.51218(2) 0.03846(12) Uani d . 1 Cu
Cu2 0.0000 0.18091(4) 0.7500 0.05902(18) Uani d S 1 Cu
Cu3 0.5000 0.63526(5) 0.7500 0.06134(18) Uani d S 1 Cu
Cl1 0.16355(6) 0.22794(7) 0.61706(6) 0.0535(2) Uani d . 1 Cl
Cl2 0.12348(6) 0.17720(6) 0.89434(6) 0.0553(2) Uani d . 1 Cl
Cl3 0.35601(9) 0.64043(12) 0.74871(14) 0.1164(5) Uani d . 1 Cl
N1 0.17978(16) 0.17912(17) 0.34962(16) 0.0370(5) Uani d . 1 N
N2 0.21024(17) 0.36749(18) 0.44526(18) 0.0410(5) Uani d . 1 N
N3 0.41216(17) 0.27198(18) 0.56550(18) 0.0439(5) Uani d . 1 N
N4 0.32272(16) 0.08647(17) 0.56185(16) 0.0363(5) Uani d . 1 N
C1 0.1576(2) 0.0842(2) 0.3048(2) 0.0440(6) Uani d . 1 C
H1 0.1803 0.0248 0.3482 0.053 Uiso calc R 1 H
C2 0.1015(2) 0.0691(3) 0.1954(2) 0.0517(7) Uani d . 1 C
H2 0.0868 0.0010 0.1672 0.062 Uiso calc R 1 H
C3 0.0688(2) 0.1550(3) 0.1307(2) 0.0509(7) Uani d . 1 C
H3 0.0321 0.1462 0.0576 0.061 Uiso calc R 1 H
C4 0.0906(2) 0.2570(2) 0.1746(2) 0.0445(7) Uani d . 1 C
C5 0.14566(19) 0.2647(2) 0.2857(2) 0.0370(6) Uani d . 1 C
C6 0.16397(19) 0.3656(2) 0.3364(2) 0.0384(6) Uani d . 1 C
C7 0.1316(2) 0.4576(2) 0.2749(2) 0.0467(7) Uani d . 1 C
C8 0.1485(2) 0.5542(2) 0.3300(3) 0.0556(8) Uani d . 1 C
H8 0.1299 0.6175 0.2921 0.067 Uiso calc R 1 H
C9 0.1928(2) 0.5555(2) 0.4404(3) 0.0579(8) Uani d . 1 C
H9 0.2033 0.6193 0.4778 0.070 Uiso calc R 1 H
C10 0.2218(2) 0.4597(2) 0.4957(3) 0.0520(7) Uani d . 1 C
H10 0.2502 0.4608 0.5705 0.062 Uiso calc R 1 H
C11 0.0606(2) 0.3525(3) 0.1134(2) 0.0541(8) Uani d . 1 C
H11 0.0264 0.3482 0.0393 0.065 Uiso calc R 1 H
C12 0.0805(2) 0.4475(3) 0.1602(3) 0.0565(8) Uani d . 1 C
H12 0.0612 0.5082 0.1181 0.068 Uiso calc R 1 H
C13 0.4563(3) 0.3646(3) 0.5725(3) 0.0622(9) Uani d . 1 C
H13 0.4166 0.4248 0.5512 0.075 Uiso calc R 1 H
C14 0.5611(3) 0.3770(3) 0.6107(3) 0.0698(10) Uani d . 1 C
H14 0.5892 0.4441 0.6159 0.084 Uiso calc R 1 H
C15 0.6202(2) 0.2903(3) 0.6397(2) 0.0591(9) Uani d . 1 C
H15 0.6892 0.2973 0.6640 0.071 Uiso calc R 1 H
C16 0.5766(2) 0.1892(2) 0.6329(2) 0.0443(6) Uani d . 1 C
C17 0.47148(19) 0.1847(2) 0.59576(18) 0.0371(6) Uani d . 1 C
C18 0.42361(18) 0.0853(2) 0.59197(17) 0.0347(5) Uani d . 1 C
C19 0.4805(2) -0.0082(2) 0.61974(17) 0.0385(6) Uani d . 1 C
C20 0.4285(2) -0.1029(2) 0.61735(19) 0.0453(7) Uani d . 1 C
H20 0.4627 -0.1669 0.6339 0.054 Uiso calc R 1 H
C21 0.3275(2) -0.1008(2) 0.5907(2) 0.0461(7) Uani d . 1 C
H21 0.2929 -0.1630 0.5908 0.055 Uiso calc R 1 H
C22 0.2767(2) -0.0047(2) 0.56342(19) 0.0427(6) Uani d . 1 C
H22 0.2080 -0.0042 0.5456 0.051 Uiso calc R 1 H
C23 0.6328(2) 0.0931(3) 0.6610(2) 0.0471(7) Uani d . 1 C
H23 0.7021 0.0959 0.6852 0.056 Uiso calc R 1 H
C24 0.5875(2) -0.0008(3) 0.65325(19) 0.0446(6) Uani d . 1 C
H24 0.6257 -0.0623 0.6697 0.054 Uiso calc R 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'
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_3
_geom_angle
_geom_angle_publ_flag
N1 Cu1 N2 . 80.12(9) y
N1 Cu1 N3 . 121.05(9) y
N1 Cu1 N4 . 95.32(8) y
N2 Cu1 N3 . 93.79(9) y
N2 Cu1 N4 . 169.29(9) y
N3 Cu1 N4 . 80.19(9) y
N1 Cu1 Cl1 . 113.90(6) y
N2 Cu1 Cl1 . 94.59(7) y
N3 Cu1 Cl1 . 125.05(7) y
N4 Cu1 Cl1 . 96.12(6) y
Cl2 Cu2 Cl2 2_556 177.44(5) y
Cl3 Cu3 Cl3 2_656 176.38(9) y
C1 N1 C5 . 117.8(2) ?
C1 N1 Cu1 . 131.81(17) ?
C5 N1 Cu1 . 110.38(17) ?
C10 N2 C6 . 118.7(2) ?
C10 N2 Cu1 . 126.5(2) ?
C6 N2 Cu1 . 114.71(18) ?
C13 N3 C17 . 117.6(3) ?
C13 N3 Cu1 . 132.2(2) ?
C17 N3 Cu1 . 110.26(17) ?
C22 N4 C18 . 118.1(2) ?
C22 N4 Cu1 . 126.98(18) ?
C18 N4 Cu1 . 114.85(17) ?
N1 C1 C2 . 123.1(3) ?
N1 C1 H1 . 118.5 ?
C2 C1 H1 . 118.5 ?
C3 C2 C1 . 119.2(3) ?
C3 C2 H2 . 120.4 ?
C1 C2 H2 . 120.4 ?
C2 C3 C4 . 119.7(3) ?
C2 C3 H3 . 120.2 ?
C4 C3 H3 . 120.2 ?
C3 C4 C5 . 117.3(3) ?
C3 C4 C11 . 124.1(3) ?
C5 C4 C11 . 118.6(3) ?
N1 C5 C4 . 123.0(3) ?
N1 C5 C6 . 117.0(2) ?
C4 C5 C6 . 120.0(2) ?
N2 C6 C7 . 122.6(3) ?
N2 C6 C5 . 117.3(2) ?
C7 C6 C5 . 120.1(2) ?
C8 C7 C6 . 117.3(3) ?
C8 C7 C12 . 124.0(3) ?
C6 C7 C12 . 118.6(3) ?
C9 C8 C7 . 119.8(3) ?
C9 C8 H8 . 120.1 ?
C7 C8 H8 . 120.1 ?
C8 C9 C10 . 119.2(3) ?
C8 C9 H9 . 120.4 ?
C10 C9 H9 . 120.4 ?
N2 C10 C9 . 122.3(3) ?
N2 C10 H10 . 118.9 ?
C9 C10 H10 . 118.9 ?
C12 C11 C4 . 121.4(3) ?
C12 C11 H11 . 119.3 ?
C4 C11 H11 . 119.3 ?
C11 C12 C7 . 121.1(3) ?
C11 C12 H12 . 119.5 ?
C7 C12 H12 . 119.5 ?
N3 C13 C14 . 123.2(3) ?
N3 C13 H13 . 118.4 ?
C14 C13 H13 . 118.4 ?
C15 C14 C13 . 119.4(3) ?
C15 C14 H14 . 120.3 ?
C13 C14 H14 . 120.3 ?
C14 C15 C16 . 119.7(3) ?
C14 C15 H15 . 120.2 ?
C16 C15 H15 . 120.2 ?
C15 C16 C17 . 117.0(3) ?
C15 C16 C23 . 123.7(3) ?
C17 C16 C23 . 119.3(3) ?
N3 C17 C16 . 123.2(3) ?
N3 C17 C18 . 117.3(2) ?
C16 C17 C18 . 119.4(2) ?
N4 C18 C19 . 123.0(2) ?
N4 C18 C17 . 116.9(2) ?
C19 C18 C17 . 120.1(2) ?
C20 C19 C18 . 116.9(2) ?
C20 C19 C24 . 124.3(3) ?
C18 C19 C24 . 118.7(3) ?
C21 C20 C19 . 119.9(3) ?
C21 C20 H20 . 120.1 ?
C19 C20 H20 . 120.1 ?
C20 C21 C22 . 119.5(3) ?
C20 C21 H21 . 120.3 ?
C22 C21 H21 . 120.3 ?
N4 C22 C21 . 122.6(3) ?
N4 C22 H22 . 118.7 ?
C21 C22 H22 . 118.7 ?
C24 C23 C16 . 121.1(3) ?
C24 C23 H23 . 119.4 ?
C16 C23 H23 . 119.4 ?
C23 C24 C19 . 121.2(3) ?
C23 C24 H24 . 119.4 ?
C19 C24 H24 . 119.4 ?
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 N1 . 2.136(2) y
Cu1 N2 . 1.989(2) y
Cu1 N3 . 2.133(2) y
Cu1 N4 . 2.000(2) y
Cu1 Cl1 . 2.2909(8) y
Cu2 Cl2 . 2.0894(7) y
Cu2 Cl2 2_556 2.0894(7) ?
Cu3 Cl3 . 2.0692(10) y
Cu3 Cl3 2_656 2.0692(10) ?
N1 C1 . 1.325(3) ?
N1 C5 . 1.353(3) ?
N2 C10 . 1.324(4) ?
N2 C6 . 1.359(3) ?
N3 C13 . 1.318(4) ?
N3 C17 . 1.361(3) ?
N4 C22 . 1.331(3) ?
N4 C18 . 1.359(3) ?
C1 C2 . 1.399(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.358(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.402(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.405(4) ?
C4 C11 . 1.431(4) ?
C5 C6 . 1.419(4) ?
C6 C7 . 1.400(4) ?
C7 C8 . 1.398(4) ?
C7 C12 . 1.440(4) ?
C8 C9 . 1.373(5) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.398(4) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.333(5) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.415(5) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.353(5) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.410(4) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.412(4) ?
C16 C23 . 1.430(4) ?
C17 C18 . 1.424(4) ?
C18 C19 . 1.407(4) ?
C19 C20 . 1.405(4) ?
C19 C24 . 1.442(4) ?
C20 C21 . 1.365(4) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.395(4) ?
C21 H21 . 0.9300 ?
C22 H22 . 0.9300 ?
C23 C24 . 1.338(4) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
