#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:40:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179122 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308471.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_4308471
loop_
_publ_author_name
'Chang-Chuan Chou'
'Chan-Cheng Su'
'Hui-Lien Tsai'
'Kwang-Hwa Lii'
_publ_section_title
;
First Example of a 2:1 Cocrystal of Mixed Cu(I)/Cu(II) Complexes and a
Novel Ferromagnetic Bis(μ-hydroxo)dicopper(II) Complex with a
Bis(pyrazol-1-yl)methane Bidentate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              628
_journal_page_last               632
_journal_paper_doi               10.1021/ic048854y
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H44 Cl4 Cu3 N20 O16'
_chemical_formula_sum            'C36 H44 Cl4 Cu3 N20 O16'
_chemical_formula_weight         1345.33
_chemical_name_systematic
;
 ?
;
_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                93.078(9)
_cell_angle_beta                 104.314(11)
_cell_angle_gamma                110.510(11)
_cell_formula_units_Z            1
_cell_length_a                   9.3397(19)
_cell_length_b                   12.4097(16)
_cell_length_c                   13.2366(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.84
_cell_measurement_theta_min      10.02
_cell_volume                     1375.6(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.1152
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5651
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.8331
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             683
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.0015(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0804P)²+0.9903P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                2436
_reflns_number_total             5403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048854ysi20040820_120349_1.cif
_cod_data_source_block           ch1862
_cod_database_code               4308471
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.0000 0.0000 0.0405(3) Uani 1 2 d S . .
Cu2 Cu 0.37209(12) 0.22235(8) 0.42788(8) 0.0644(3) Uani 1 1 d . . .
N1 N 0.3031(6) -0.0272(4) 0.0435(4) 0.0417(13) Uani 1 1 d . . .
N2 N 0.1927(6) -0.1340(4) 0.0365(4) 0.0403(13) Uani 1 1 d . . .
N3 N 0.3543(6) -0.2434(4) 0.0349(4) 0.0448(13) Uani 1 1 d . . .
N4 N 0.4929(6) -0.1567(4) 0.0358(4) 0.0445(13) Uani 1 1 d . . .
N5 N 0.5948(7) 0.3534(5) 0.4903(5) 0.0573(16) Uani 1 1 d . . .
N6 N 0.6788(7) 0.3939(5) 0.4208(5) 0.0538(15) Uani 1 1 d . . .
N7 N 0.4808(7) 0.3331(5) 0.2552(4) 0.0485(14) Uani 1 1 d . . .
N8 N 0.3454(7) 0.2831(5) 0.2836(4) 0.0475(14) Uani 1 1 d . . .
N9 N 0.3975(7) 0.0688(6) 0.3952(5) 0.0596(17) Uani 1 1 d . . .
N10 N 0.2172(8) 0.1979(6) 0.5047(5) 0.0606(16) Uani 1 1 d . . .
C1 C 0.2642(8) 0.0452(5) 0.1006(5) 0.0452(16) Uani 1 1 d . . .
C2 C 0.1259(8) -0.0165(6) 0.1262(6) 0.0542(19) Uani 1 1 d . . .
C3 C 0.0849(7) -0.1292(6) 0.0860(6) 0.0479(17) Uani 1 1 d . . .
C4 C 0.2036(8) -0.2357(5) -0.0177(5) 0.0437(16) Uani 1 1 d . . .
C5 C 0.3826(10) -0.3271(6) 0.0855(6) 0.059(2) Uani 1 1 d . . .
C6 C 0.5434(11) -0.2944(7) 0.1206(7) 0.069(2) Uani 1 1 d . . .
C7 C 0.6078(8) -0.1884(6) 0.0876(6) 0.0551(19) Uani 1 1 d . . .
C8 C 0.6679(11) 0.4349(8) 0.5750(6) 0.075(2) Uani 1 1 d . . .
C9 C 0.7968(11) 0.5247(7) 0.5601(7) 0.080(3) Uani 1 1 d . . .
C10 C 0.7981(9) 0.4970(7) 0.4620(8) 0.070(2) Uani 1 1 d . . .
C11 C 0.6286(9) 0.3266(6) 0.3178(6) 0.0556(19) Uani 1 1 d . . .
C12 C 0.4527(12) 0.3835(6) 0.1681(6) 0.069(2) Uani 1 1 d . . .
C13 C 0.2969(12) 0.3661(7) 0.1392(7) 0.076(3) Uani 1 1 d . . .
C14 C 0.2349(9) 0.3043(7) 0.2139(7) 0.066(2) Uani 1 1 d . . .
C15 C 0.4011(8) -0.0167(7) 0.3663(6) 0.0523(18) Uani 1 1 d . . .
C16 C 0.5943(10) 0.1284(7) 0.6714(7) 0.072(2) Uani 1 1 d . . .
C17 C 0.1201(10) 0.1757(7) 0.5453(6) 0.062(2) Uani 1 1 d . . .
C18 C -0.0049(11) 0.1445(8) 0.5975(8) 0.087(3) Uani 1 1 d . . .
Cl1 Cl 0.79484(19) 0.09780(15) 0.27104(14) 0.0486(4) Uani 1 1 d . . .
Cl2 Cl -0.0606(2) -0.43996(15) 0.17131(15) 0.0568(5) Uani 1 1 d . . .
O1 O 0.6462(5) 0.0862(4) 0.1982(4) 0.0611(13) Uani 1 1 d . . .
O2 O 0.8874(8) 0.0704(8) 0.2145(6) 0.133(3) Uani 1 1 d . . .
O3 O 0.8753(8) 0.2128(6) 0.3204(7) 0.131(3) Uani 1 1 d . . .
O4 O 0.7676(9) 0.0247(9) 0.3428(7) 0.160(4) Uani 1 1 d . . .
O5 O -0.1378(19) -0.5555(13) 0.1777(12) 0.092(5) Uiso 0.50 1 d P . .
O6 O 0.073(2) -0.3524(14) 0.2381(14) 0.121(5) Uiso 0.50 1 d P . .
O7 O -0.0384(19) -0.4480(13) 0.0641(12) 0.114(5) Uiso 0.50 1 d P . .
O8 O -0.182(3) -0.3963(19) 0.160(2) 0.170(8) Uiso 0.50 1 d P . .
O5' O -0.0644(18) -0.5534(12) 0.1927(11) 0.082(4) Uiso 0.50 1 d P . .
O6' O 0.1057(19) -0.3779(14) 0.1854(13) 0.114(5) Uiso 0.50 1 d P . .
O7' O -0.154(2) -0.4155(15) 0.0808(15) 0.128(5) Uiso 0.50 1 d P . .
O8' O -0.102(2) -0.3950(15) 0.2614(14) 0.133(6) Uiso 0.50 1 d P . .
H1 H 0.3226 0.1311 0.1194 0.053 Uiso 1 1 d . . .
H2 H 0.0690 0.0152 0.1689 0.062 Uiso 1 1 d . . .
H3 H -0.0066 -0.1986 0.0916 0.056 Uiso 1 1 d . . .
H4A H 0.1926 -0.2288 -0.0995 0.055 Uiso 1 1 d . . .
H4B H 0.1050 -0.3142 -0.0125 0.055 Uiso 1 1 d . . .
H5 H 0.3019 -0.3987 0.0978 0.061 Uiso 1 1 d . . .
H6 H 0.6027 -0.3383 0.1621 0.074 Uiso 1 1 d . . .
H7 H 0.7229 -0.1428 0.1010 0.063 Uiso 1 1 d . . .
H8 H 0.6307 0.4329 0.6402 0.077 Uiso 1 1 d . . .
H9 H 0.8734 0.5922 0.6146 0.080 Uiso 1 1 d . . .
H10 H 0.8756 0.5469 0.4251 0.078 Uiso 1 1 d . . .
H11A H 0.7218 0.3599 0.2793 0.062 Uiso 1 1 d . . .
H11B H 0.6106 0.2371 0.3267 0.062 Uiso 1 1 d . . .
H12 H 0.5331 0.4240 0.1305 0.076 Uiso 1 1 d . . .
H13 H -0.2413 -0.3920 -0.0792 0.080 Uiso 1 1 d . . .
H14 H 0.1208 0.2807 0.2151 0.075 Uiso 1 1 d . . .
H16A H 0.5134 0.1532 0.6091 0.078 Uiso 1 1 d . . .
H16B H 0.5517 0.1250 0.7403 0.078 Uiso 1 1 d . . .
H16C H 0.2870 -0.1918 0.3123 0.078 Uiso 1 1 d . . .
H18A H -0.1233 0.1180 0.5441 0.097 Uiso 1 1 d . . .
H18B H -0.0106 -0.2181 0.3436 0.097 Uiso 1 1 d . . .
H18C H 0.0103 0.0745 0.6384 0.097 Uiso 1 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'
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'
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'
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
_geom_angle_publ_flag
N1 Cu1 N1 180.0(3) . 2_655 ?
N1 Cu1 N4 91.2(2) . 2_655 ?
N1 Cu1 N4 88.8(2) 2_655 2_655 ?
N1 Cu1 N4 88.8(2) . . ?
N1 Cu1 N4 91.2(2) 2_655 . ?
N4 Cu1 N4 180.0(5) 2_655 . ?
N10 Cu2 N9 108.9(3) . . ?
N10 Cu2 N5 118.9(3) . . ?
N9 Cu2 N5 109.5(2) . . ?
N10 Cu2 N8 122.6(2) . . ?
N9 Cu2 N8 103.5(2) . . ?
N5 Cu2 N8 91.5(2) . . ?
C1 N1 N2 105.7(5) . . ?
C1 N1 Cu1 130.1(4) . . ?
N2 N1 Cu1 123.1(4) . . ?
N1 N2 C3 110.8(5) . . ?
N1 N2 C4 120.1(5) . . ?
C3 N2 C4 129.1(5) . . ?
C5 N3 N4 111.0(6) . . ?
C5 N3 C4 129.4(6) . . ?
N4 N3 C4 119.7(5) . . ?
C7 N4 N3 105.7(5) . . ?
C7 N4 Cu1 130.2(4) . . ?
N3 N4 Cu1 121.9(4) . . ?
C8 N5 N6 103.8(6) . . ?
C8 N5 Cu2 136.8(6) . . ?
N6 N5 Cu2 116.3(4) . . ?
C10 N6 N5 111.3(7) . . ?
C10 N6 C11 130.1(7) . . ?
N5 N6 C11 118.5(6) . . ?
C12 N7 N8 111.0(6) . . ?
C12 N7 C11 129.9(7) . . ?
N8 N7 C11 119.1(5) . . ?
C14 N8 N7 104.9(6) . . ?
C14 N8 Cu2 138.0(5) . . ?
N7 N8 Cu2 116.2(4) . . ?
C15 N9 Cu2 172.4(6) . . ?
C17 N10 Cu2 174.9(7) . . ?
N1 C1 C2 109.8(6) . . ?
C3 C2 C1 106.0(6) . . ?
N2 C3 C2 107.6(6) . . ?
N3 C4 N2 108.3(5) . . ?
N3 C5 C6 107.0(6) . . ?
C5 C6 C7 106.3(7) . . ?
N4 C7 C6 110.1(6) . . ?
N5 C8 C9 111.5(8) . . ?
C10 C9 C8 105.4(7) . . ?
C9 C10 N6 108.0(7) . . ?
N6 C11 N7 110.3(5) . . ?
C13 C12 N7 107.5(7) . . ?
C12 C13 C14 105.2(7) . . ?
N8 C14 C13 111.4(8) . . ?
N9 C15 C16 179.9(11) . 2_656 ?
N10 C17 C18 178.8(9) . . ?
O4 Cl1 O2 110.1(6) . . ?
O4 Cl1 O3 111.0(6) . . ?
O2 Cl1 O3 108.1(5) . . ?
O4 Cl1 O1 109.8(4) . . ?
O2 Cl1 O1 108.3(4) . . ?
O3 Cl1 O1 109.4(4) . . ?
O5 Cl2 O6 132.3(9) . . ?
O5 Cl2 O8 102.7(11) . . ?
O6 Cl2 O8 104.5(12) . . ?
O5 Cl2 O7' 106.7(9) . . ?
O6 Cl2 O7' 120.8(10) . . ?
O8 Cl2 O7' 49.3(10) . . ?
O5 Cl2 O6' 128.3(9) . . ?
O6 Cl2 O6' 37.8(8) . . ?
O8 Cl2 O6' 128.7(11) . . ?
O7' Cl2 O6' 111.1(10) . . ?
O5 Cl2 O5' 26.7(7) . . ?
O6 Cl2 O5' 111.3(9) . . ?
O8 Cl2 O5' 128.7(11) . . ?
O7' Cl2 O5' 126.4(9) . . ?
O6' Cl2 O5' 101.6(9) . . ?
O5 Cl2 O8' 94.6(9) . . ?
O6 Cl2 O8' 69.9(9) . . ?
O8 Cl2 O8' 56.5(10) . . ?
O7' Cl2 O8' 105.4(10) . . ?
O6' Cl2 O8' 107.6(10) . . ?
O5' Cl2 O8' 103.5(9) . . ?
O5 Cl2 O7 101.6(9) . . ?
O6 Cl2 O7 108.7(9) . . ?
O8 Cl2 O7 104.0(12) . . ?
O7' Cl2 O7 54.9(8) . . ?
O6' Cl2 O7 74.3(9) . . ?
O5' Cl2 O7 98.1(8) . . ?
O8' Cl2 O7 157.3(9) . . ?
O5' O5 Cl2 82(2) . . ?
O6' O6 Cl2 73.8(16) . . ?
O6' O6 O8' 131(2) . . ?
Cl2 O6 O8' 57.7(9) . . ?
O7' O7 Cl2 59.7(10) . . ?
O7' O7 O6' 97.3(14) . . ?
Cl2 O7 O6' 51.3(7) . . ?
O7' O8 O8' 130(2) . . ?
O7' O8 Cl2 65.9(15) . . ?
O8' O8 Cl2 64.6(13) . . ?
O5 O5' Cl2 71(2) . . ?
O6 O6' Cl2 68.5(16) . . ?
O6 O6' O7 118(2) . . ?
Cl2 O6' O7 54.3(7) . . ?
O8 O7' O7 130(2) . . ?
O8 O7' Cl2 64.9(15) . . ?
O7 O7' Cl2 65.4(10) . . ?
O8 O8' Cl2 58.9(12) . . ?
O8 O8' O6 93.8(15) . . ?
Cl2 O8' O6 52.4(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.985(5) . ?
Cu1 N1 1.985(5) 2_655 ?
Cu1 N4 2.009(5) 2_655 ?
Cu1 N4 2.009(5) . ?
Cu2 N10 1.916(6) . ?
Cu2 N9 2.038(7) . ?
Cu2 N5 2.071(6) . ?
Cu2 N8 2.080(6) . ?
N1 C1 1.342(7) . ?
N1 N2 1.345(6) . ?
N2 C3 1.346(7) . ?
N2 C4 1.464(8) . ?
N3 C5 1.333(8) . ?
N3 N4 1.360(7) . ?
N3 C4 1.446(8) . ?
N4 C7 1.318(8) . ?
N5 C8 1.328(9) . ?
N5 N6 1.358(8) . ?
N6 C10 1.342(9) . ?
N6 C11 1.436(9) . ?
N7 C12 1.353(9) . ?
N7 N8 1.355(7) . ?
N7 C11 1.456(9) . ?
N8 C14 1.316(9) . ?
N9 C15 1.124(9) . ?
N10 C17 1.126(9) . ?
C1 C2 1.386(9) . ?
C2 C3 1.352(9) . ?
C5 C6 1.357(11) . ?
C6 C7 1.385(10) . ?
C8 C9 1.390(12) . ?
C9 C10 1.329(11) . ?
C12 C13 1.344(12) . ?
C13 C14 1.398(11) . ?
C15 C16 1.466(11) 2_656 ?
C16 C15 1.466(11) 2_656 ?
C17 C18 1.449(11) . ?
Cl1 O4 1.356(7) . ?
Cl1 O2 1.386(6) . ?
Cl1 O3 1.391(6) . ?
Cl1 O1 1.436(5) . ?
Cl2 O5 1.379(15) . ?
Cl2 O6 1.385(17) . ?
Cl2 O8 1.40(2) . ?
Cl2 O7' 1.412(18) . ?
Cl2 O6' 1.430(16) . ?
Cl2 O5' 1.441(14) . ?
Cl2 O8' 1.479(18) . ?
Cl2 O7 1.487(15) . ?
O5 O5' 0.655(18) . ?
O6 O6' 0.912(19) . ?
O6 O8' 1.64(2) . ?
O7 O7' 1.338(19) . ?
O7 O6' 1.76(2) . ?
O8 O7' 1.17(2) . ?
O8 O8' 1.36(2) . ?
