#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/15/2201505.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_2201505
loop_
_publ_author_name
'Valdés-Martínez, Jesús'
'Salazar-Mendoza, Domingo'
'Toscano, Rubén A.'
_publ_section_title
;
 Di-μ-chloro-bis[(2,2':6,2''-terpyridine)copper(II)] diperchlorate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m712
_journal_page_last               m714
_journal_paper_doi               10.1107/S1600536802020470
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Cu2 Cl2 (C15 H11 N3)2] (Cl O4)2'
_chemical_formula_moiety         'C30 H22 Cl2 Cu2 N6, 2(Cl O4)'
_chemical_formula_sum            'C30 H22 Cl4 Cu2 N6 O8'
_chemical_formula_weight         863.42
_chemical_name_systematic
;
Di-μ-chloro-bis[(2,2':6,2''-terpyridine)copper(II)] diperchlorate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4390(10)
_cell_length_b                   24.387(4)
_cell_length_c                   9.1960(10)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      4.66
_cell_volume                     1605.6(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1993)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics
'PLATON (Spek, 1999) and MERCURY (Version 1.1; Bruno et al., 2002)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Siemens P4/PC'
_diffrn_measurement_method       ω-2θ
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3043
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        3.48
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated pyramid'
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.654
_refine_ls_extinction_coef       0.0094(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0602
_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)+(0.0670P)²+2.0508P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1726
_reflns_number_gt                1856
_reflns_number_total             2818
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh6012.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2201505
_cod_database_fobs_code          2201505
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu 0.23258(13) 0.01644(4) 0.03173(10) 0.0379(3) Uani d . 1 . . Cu
Cl1 0.0204(3) 0.00230(8) -0.1879(2) 0.0450(5) Uani d . 1 . . Cl
N1 0.4336(9) 0.0292(3) 0.2129(7) 0.0411(15) Uani d . 1 . . N
C2 0.5324(10) -0.0141(3) 0.2807(8) 0.0402(16) Uani d . 1 . . C
C3 0.6779(12) -0.0047(4) 0.4129(10) 0.058(2) Uani d . 1 . . C
H3 0.7493 -0.0352 0.4641 0.069 Uiso d R 1 . . H
C4 0.7176(13) 0.0467(4) 0.4679(10) 0.061(3) Uani d . 1 . . C
H4 0.8197 0.0529 0.5560 0.073 Uiso d R 1 . . H
C5 0.6073(13) 0.0909(4) 0.3949(9) 0.056(2) Uani d . 1 . . C
H5 0.6293 0.1275 0.4343 0.067 Uiso d R 1 . . H
C6 0.4651(11) 0.0807(3) 0.2633(9) 0.0426(17) Uani d . 1 . . C
N11 0.3365(9) -0.0608(3) 0.0675(7) 0.0422(14) Uani d . 1 . . N
C12 0.4718(11) -0.0661(3) 0.2019(9) 0.0436(17) Uani d . 1 . . C
C13 0.5396(13) -0.1173(4) 0.2539(12) 0.059(2) Uani d . 1 . . C
H13 0.6324 -0.1207 0.3491 0.071 Uiso d R 1 . . H
C14 0.4735(15) -0.1640(4) 0.1689(12) 0.063(3) Uani d . 1 . . C
H14 0.5202 -0.1997 0.2044 0.075 Uiso d R 1 . . H
C15 0.3426(15) -0.1578(4) 0.0344(12) 0.063(2) Uani d . 1 . . C
H15 0.2960 -0.1893 -0.0267 0.076 Uiso d R 1 . . H
C16 0.2767(13) -0.1065(3) -0.0132(10) 0.0477(19) Uani d . 1 . . C
H16 0.1835 -0.1028 -0.1081 0.057 Uiso d R 1 . . H
N21 0.2278(10) 0.0987(2) 0.0379(8) 0.0435(15) Uani d . 1 . . N
C22 0.3441(11) 0.1211(3) 0.1650(9) 0.0435(18) Uani d . 1 . . C
C23 0.3512(14) 0.1773(3) 0.1895(12) 0.059(2) Uani d . 1 . . C
H23 0.4363 0.1923 0.2783 0.071 Uiso d R 1 . . H
C24 0.2385(18) 0.2100(4) 0.0881(14) 0.076(3) Uani d . 1 . . C
H24 0.2360 0.2486 0.1079 0.091 Uiso d R 1 . . H
C25 0.1264(17) 0.1892(4) -0.0421(14) 0.077(3) Uani d . 1 . . C
H25 0.0532 0.2132 -0.1183 0.093 Uiso d R 1 . . H
C26 0.1205(12) 0.1327(4) -0.0632(10) 0.051(2) Uani d . 1 . . C
H26 0.0374 0.1174 -0.1527 0.061 Uiso d R 1 . . H
Cl2 0.4707(3) -0.32610(8) 0.0479(3) 0.0557(6) Uani d . 1 . . Cl
O1 0.4210(13) -0.3781(3) 0.0939(12) 0.096(3) Uani d . 1 . . O
O2 0.5406(15) -0.3342(4) -0.0808(9) 0.097(3) Uani d . 1 . . O
O3 0.6117(14) -0.3025(3) 0.1638(10) 0.095(3) Uani d . 1 . . O
O4 0.3109(14) -0.2911(3) 0.0107(12) 0.101(3) Uani d . 1 . . O
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'
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_3
_geom_angle
_geom_angle_publ_flag
N1 Cu N21 . 80.3(3) yes
N1 Cu N11 . 80.7(3) yes
N21 Cu N11 . 158.8(3) yes
N1 Cu Cl1 . 174.9(2) yes
N21 Cu Cl1 . 99.6(2) yes
N11 Cu Cl1 . 98.5(2) yes
N1 Cu Cl1 3 93.2(2) yes
N21 Cu Cl1 3 97.7(2) no
N11 Cu Cl1 3 92.67(19) no
Cl1 Cu Cl1 3 91.80(7) yes
Cu Cl1 Cu 3 88.20(7) yes
C6 N1 C2 . 123.8(7) no
C6 N1 Cu . 118.0(5) no
C2 N1 Cu . 118.2(5) no
N1 C2 C3 . 118.0(8) no
N1 C2 C12 . 113.2(6) no
C3 C2 C12 . 128.8(8) no
C4 C3 C2 . 120.7(9) no
C4 C3 H3 . 119.9 no
C2 C3 H3 . 119.4 no
C3 C4 C5 . 119.4(8) no
C3 C4 H4 . 120.2 no
C5 C4 H4 . 120.4 no
C6 C5 C4 . 118.8(8) no
C6 C5 H5 . 120.3 no
C4 C5 H5 . 120.9 no
N1 C6 C5 . 119.2(8) no
N1 C6 C22 . 113.4(7) no
C5 C6 C22 . 127.3(8) no
C16 N11 C12 . 118.0(7) no
C16 N11 Cu . 128.7(6) no
C12 N11 Cu . 112.9(5) no
N11 C12 C13 . 120.5(8) no
N11 C12 C2 . 114.4(7) no
C13 C12 C2 . 125.1(8) no
C12 C13 C14 . 120.3(9) no
C12 C13 H13 . 119.7 no
C14 C13 H13 . 120.0 no
C15 C14 C13 . 118.4(8) no
C15 C14 H14 . 121.0 no
C13 C14 H14 . 120.6 no
C14 C15 C16 . 119.9(9) no
C14 C15 H15 . 119.9 no
C16 C15 H15 . 120.1 no
N11 C16 C15 . 122.9(9) no
N11 C16 H16 . 118.3 no
C15 C16 H16 . 118.9 no
C26 N21 C22 . 117.9(7) no
C26 N21 Cu . 127.7(6) no
C22 N21 Cu . 114.3(5) no
N21 C22 C23 . 121.4(8) no
N21 C22 C6 . 113.5(6) no
C23 C22 C6 . 124.9(8) no
C24 C23 C22 . 119.2(9) no
C24 C23 H23 . 120.7 no
C22 C23 H23 . 120.1 no
C23 C24 C25 . 120.7(9) no
C23 C24 H24 . 119.7 no
C25 C24 H24 . 119.6 no
C24 C25 C26 . 118.8(10) no
C24 C25 H25 . 120.5 no
C26 C25 H25 . 120.7 no
N21 C26 C25 . 121.8(9) no
N21 C26 H26 . 118.8 no
C25 C26 H26 . 119.4 no
O3 Cl2 O1 . 110.1(6) no
O3 Cl2 O4 . 109.9(6) no
O1 Cl2 O4 . 109.8(6) no
O3 Cl2 O2 . 108.7(6) no
O1 Cl2 O2 . 107.9(6) no
O4 Cl2 O2 . 110.5(6) no
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 N1 . 1.938(6) yes
Cu N21 . 2.008(6) yes
Cu N11 . 2.028(6) yes
Cu Cl1 . 2.227(2) yes
Cu Cl1 3 2.698(2) yes
Cl1 Cu 3 2.698(2) no
N1 C6 . 1.338(10) no
N1 C2 . 1.339(10) no
C2 C3 . 1.410(11) no
C2 C12 . 1.470(11) no
C3 C4 . 1.354(14) no
C3 H3 . 0.9600 no
C4 C5 . 1.410(14) no
C4 H4 . 0.9600 no
C5 C6 . 1.396(11) no
C5 H5 . 0.9599 no
C6 C22 . 1.469(11) no
N11 C16 . 1.346(10) no
N11 C12 . 1.372(10) no
C12 C13 . 1.383(11) no
C13 C14 . 1.393(14) no
C13 H13 . 0.9600 no
C14 C15 . 1.359(15) no
C14 H14 . 0.9599 no
C15 C16 . 1.371(11) no
C15 H15 . 0.9600 no
C16 H16 . 0.9600 no
N21 C26 . 1.335(10) no
N21 C22 . 1.364(10) no
C22 C23 . 1.387(11) no
C23 C24 . 1.336(15) no
C23 H23 . 0.9600 no
C24 C25 . 1.357(16) no
C24 H24 . 0.9599 no
C25 C26 . 1.393(14) no
C25 H25 . 0.9599 no
C26 H26 . 0.9600 no
Cl2 O3 . 1.400(8) no
Cl2 O1 . 1.417(8) no
Cl2 O4 . 1.427(9) no
Cl2 O2 . 1.430(10) no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N21 Cu Cl1 Cu . 3 -98.1(2) no
N11 Cu Cl1 Cu . 3 92.97(19) no
Cl1 Cu Cl1 Cu 3 3 0.0 no
N21 Cu N1 C6 . . 5.3(6) no
N11 Cu N1 C6 . . 175.9(6) no
Cl1 Cu N1 C6 3 . -92.0(6) no
N21 Cu N1 C2 . . -174.9(6) no
N11 Cu N1 C2 . . -4.4(6) no
Cl1 Cu N1 C2 3 . 87.8(6) no
C6 N1 C2 C3 . . 0.1(11) no
Cu N1 C2 C3 . . -179.7(5) no
C6 N1 C2 C12 . . -179.2(7) no
Cu N1 C2 C12 . . 1.0(9) no
N1 C2 C3 C4 . . -0.9(12) no
C12 C2 C3 C4 . . 178.2(8) no
C2 C3 C4 C5 . . 2.3(14) no
C3 C4 C5 C6 . . -2.9(14) no
C2 N1 C6 C5 . . -0.7(12) no
Cu N1 C6 C5 . . 179.1(6) no
C2 N1 C6 C22 . . 177.1(7) no
Cu N1 C6 C22 . . -3.2(9) no
C4 C5 C6 N1 . . 2.0(13) no
C4 C5 C6 C22 . . -175.4(9) no
N1 Cu N11 C16 . . 179.2(8) no
N21 Cu N11 C16 . . -154.3(8) no
Cl1 Cu N11 C16 . . -5.9(7) no
Cl1 Cu N11 C16 3 . 86.4(7) no
N1 Cu N11 C12 . . 7.0(5) no
N21 Cu N11 C12 . . 33.5(11) no
Cl1 Cu N11 C12 . . -178.1(5) no
Cl1 Cu N11 C12 3 . -85.9(5) no
C16 N11 C12 C13 . . -1.9(12) no
Cu N11 C12 C13 . . 171.2(7) no
C16 N11 C12 C2 . . 178.5(7) no
Cu N11 C12 C2 . . -8.4(8) no
N1 C2 C12 N11 . . 5.0(10) yes
C3 C2 C12 N11 . . -174.1(7) no
N1 C2 C12 C13 . . -174.5(8) no
C3 C2 C12 C13 . . 6.3(14) no
N11 C12 C13 C14 . . 1.2(14) no
C2 C12 C13 C14 . . -179.3(9) no
C12 C13 C14 C15 . . 0.4(16) no
C13 C14 C15 C16 . . -1.1(16) no
C12 N11 C16 C15 . . 1.2(13) no
Cu N11 C16 C15 . . -170.7(7) no
C14 C15 C16 N11 . . 0.3(16) no
N1 Cu N21 C26 . . 176.4(8) no
N11 Cu N21 C26 . . 149.9(8) no
Cl1 Cu N21 C26 . . 1.6(8) no
Cl1 Cu N21 C26 3 . -91.6(8) no
N1 Cu N21 C22 . . -6.5(6) no
N11 Cu N21 C22 . . -33.1(12) no
Cl1 Cu N21 C22 . . 178.6(6) no
Cl1 Cu N21 C22 3 . 85.4(6) no
C26 N21 C22 C23 . . 0.1(13) no
Cu N21 C22 C23 . . -177.2(7) no
C26 N21 C22 C6 . . -176.0(8) no
Cu N21 C22 C6 . . 6.7(9) no
N1 C6 C22 N21 . . -2.5(11) yes
C5 C6 C22 N21 . . 175.1(9) no
N1 C6 C22 C23 . . -178.4(8) no
C5 C6 C22 C23 . . -0.9(15) no
N21 C22 C23 C24 . . 1.6(15) no
C6 C22 C23 C24 . . 177.3(10) no
C22 C23 C24 C25 . . -4.1(18) no
C23 C24 C25 C26 . . 4.8(19) no
C22 N21 C26 C25 . . 0.6(14) no
Cu N21 C26 C25 . . 177.5(8) no
C24 C25 C26 N21 . . -3.0(17) no
