#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:42:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179258 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/78/4317838.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_4317838
loop_
_publ_author_name
'Panagiotis A. Angaridis'
'Peter Baran'
'R. Boča'
'Francisco Cervantes-Lee'
'W. Haase'
'Gellert Mezei'
'Raphael G. Raptis'
'R. Werner'
_publ_section_title
;
 Synthesis and Structural Characterization of Trinuclear CuII-Pyrazolato
 Complexes Containing μ3-OH, μ3-O, and μ3-Cl Ligands. Magnetic
 Susceptibility Study of [PPN]2[(μ3-O)Cu3(μ-pz)3Cl3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2219
_journal_page_last               2228
_journal_paper_doi               10.1021/ic010670l
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Et3NH[Cu3(mu-OH)(mu-pz)3Cl3(pzH)]
_chemical_formula_sum            'C18 H30 Cl3 Cu3 N9 O'
_chemical_formula_weight         685.48
_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                66.475(3)
_cell_angle_beta                 64.279(3)
_cell_angle_gamma                80.183(3)
_cell_formula_units_Z            2
_cell_length_a                   11.498(2)
_cell_length_b                   11.499(2)
_cell_length_c                   12.186(2)
_cell_measurement_temperature    298(2)
_cell_volume                     1330.9(4)
_computing_cell_refinement       'BRUKER SMART-NT V5.0'
_computing_data_collection       'BRUKER SMART-NT V5.0'
_computing_data_reduction        'BRUKER SAINT-NT V5/6.0'
_computing_molecular_graphics    'BRUKER SHELXTL-NT V5.1'
_computing_publication_material  'BRUKER SHELXTL-NT V5.1'
_computing_structure_refinement  'BRUKER SHELXTL-NT V5.1'
_computing_structure_solution    'BRUKER SHELXTL-NT V5.1'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS SMART CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5792
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.706
_exptl_absorpt_correction_T_max  0.6553
_exptl_absorpt_correction_T_min  0.4595
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'plum blue'
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3815
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          2.037
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0755P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                2717
_reflns_number_total             3815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010670l.cif
_cod_data_source_block           pba018
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1331.0(5)
_cod_database_code               4317838
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 -0.22473(7) 0.77069(7) 0.43209(8) 0.0529(3) Uani 1 1 d . . .
Cu2 Cu 0.04342(8) 0.59538(7) 0.33101(8) 0.0561(3) Uani 1 1 d . . .
Cu3 Cu 0.06724(7) 0.88617(7) 0.29890(7) 0.0461(2) Uani 1 1 d . . .
O1 O -0.0409(4) 0.7271(3) 0.4103(4) 0.0423(10) Uani 1 1 d D . .
H1O1 H -0.048(4) 0.699(4) 0.494(2) 0.015(12) Uiso 1 1 d D . .
Cl1 Cl -0.43964(18) 0.8029(2) 0.4973(3) 0.1030(8) Uani 1 1 d . . .
Cl2 Cl 0.1397(2) 0.41722(17) 0.28405(19) 0.0811(6) Uani 1 1 d . . .
Cl3 Cl 0.00761(17) 0.85060(16) 0.12523(16) 0.0613(5) Uani 1 1 d . . .
N1 N -0.2316(5) 0.6240(5) 0.3957(5) 0.0508(13) Uani 1 1 d . . .
N2 N -0.1272(5) 0.5518(5) 0.3610(5) 0.0576(15) Uani 1 1 d . . .
N3 N 0.2081(5) 0.6558(5) 0.2943(5) 0.0517(13) Uani 1 1 d . . .
N4 N 0.2215(5) 0.7810(5) 0.2674(5) 0.0521(13) Uani 1 1 d . . .
N5 N -0.0777(5) 0.9774(4) 0.3855(5) 0.0468(13) Uani 1 1 d . . .
N6 N -0.1999(5) 0.9267(5) 0.4457(5) 0.0515(13) Uani 1 1 d . . .
N7 N 0.1618(5) 1.0498(5) 0.1681(5) 0.0515(13) Uani 1 1 d . . .
N8 N 0.1454(5) 1.1101(5) 0.0553(5) 0.0550(14) Uani 1 1 d . . .
H8N H 0.1019 1.0799 0.0303 0.066 Uiso 1 1 calc R . .
N9 N 0.7372(6) 0.2178(6) 0.0913(6) 0.0655(17) Uani 1 1 d . . .
H9N H 0.800(7) 0.202(7) 0.021(7) 0.079 Uiso 1 1 calc . . .
C1 C -0.1644(8) 0.4553(7) 0.3469(8) 0.079(2) Uani 1 1 d . . .
H1 H -0.1101 0.3917 0.3230 0.095 Uiso 1 1 calc R . .
C2 C -0.2926(8) 0.4643(7) 0.3725(8) 0.078(2) Uani 1 1 d . . .
H2 H -0.3425 0.4103 0.3701 0.094 Uiso 1 1 calc R . .
C3 C -0.3309(7) 0.5709(7) 0.4026(7) 0.067(2) Uani 1 1 d . . .
H3 H -0.4146 0.6024 0.4249 0.081 Uiso 1 1 calc R . .
C4 C 0.3437(7) 0.8014(7) 0.2385(7) 0.066(2) Uani 1 1 d . . .
H4 H 0.3776 0.8792 0.2172 0.079 Uiso 1 1 calc R . .
C5 C 0.4120(7) 0.6906(8) 0.2448(8) 0.074(2) Uani 1 1 d . . .
H5 H 0.4995 0.6790 0.2269 0.089 Uiso 1 1 calc R . .
C6 C 0.3250(7) 0.6016(7) 0.2824(7) 0.068(2) Uani 1 1 d . . .
H6 H 0.3429 0.5159 0.2979 0.082 Uiso 1 1 calc R . .
C7 C -0.2813(7) 1.0049(6) 0.5008(7) 0.0602(18) Uani 1 1 d . . .
H7 H -0.3703 0.9937 0.5459 0.072 Uiso 1 1 calc R . .
C8 C -0.2138(7) 1.1039(6) 0.4807(6) 0.0603(18) Uani 1 1 d . . .
H8 H -0.2467 1.1706 0.5103 0.072 Uiso 1 1 calc R . .
C9 C -0.0881(7) 1.0842(6) 0.4081(7) 0.0577(18) Uani 1 1 d . . .
H9 H -0.0197 1.1374 0.3786 0.069 Uiso 1 1 calc R . .
C10 C 0.2048(7) 1.2221(7) -0.0122(7) 0.069(2) Uani 1 1 d . . .
H10 H 0.2068 1.2792 -0.0927 0.082 Uiso 1 1 calc R . .
C11 C 0.2617(7) 1.2375(7) 0.0574(8) 0.074(2) Uani 1 1 d . . .
H11 H 0.3110 1.3063 0.0344 0.089 Uiso 1 1 calc R . .
C12 C 0.2317(7) 1.1303(7) 0.1696(7) 0.0653(19) Uani 1 1 d . . .
H12 H 0.2566 1.1160 0.2371 0.078 Uiso 1 1 calc R . .
C13 C 0.8069(9) 0.2583(9) 0.1499(8) 0.093(3) Uani 1 1 d . . .
H13A H 0.8641 0.1908 0.1750 0.112 Uiso 1 1 calc R . .
H13B H 0.7444 0.2720 0.2284 0.112 Uiso 1 1 calc R . .
C14 C 0.8849(10) 0.3787(9) 0.0562(10) 0.116(3) Uani 1 1 d . . .
H14A H 0.9485 0.3651 -0.0208 0.175 Uiso 1 1 calc R . .
H14B H 0.9272 0.4010 0.0979 0.175 Uiso 1 1 calc R . .
H14C H 0.8285 0.4462 0.0320 0.175 Uiso 1 1 calc R . .
C15 C 0.6522(9) 0.3145(9) 0.0386(9) 0.100(3) Uani 1 1 d . . .
H15A H 0.6185 0.2814 -0.0037 0.120 Uiso 1 1 calc R . .
H15B H 0.7030 0.3896 -0.0271 0.120 Uiso 1 1 calc R . .
C16 C 0.5402(10) 0.3515(11) 0.1441(10) 0.139(4) Uani 1 1 d . . .
H16A H 0.4780 0.2838 0.1968 0.208 Uiso 1 1 calc R . .
H16B H 0.5003 0.4269 0.1040 0.208 Uiso 1 1 calc R . .
H16C H 0.5714 0.3672 0.1984 0.208 Uiso 1 1 calc R . .
C17 C 0.6728(9) 0.0927(9) 0.1845(9) 0.098(3) Uani 1 1 d . . .
H17A H 0.7380 0.0333 0.2049 0.117 Uiso 1 1 calc R . .
H17B H 0.6116 0.1030 0.2652 0.117 Uiso 1 1 calc R . .
C18 C 0.6039(9) 0.0347(10) 0.1408(10) 0.115(3) Uani 1 1 d . . .
H18A H 0.5249 0.0797 0.1433 0.172 Uiso 1 1 calc R . .
H18B H 0.5848 -0.0524 0.1978 0.172 Uiso 1 1 calc R . .
H18C H 0.6573 0.0392 0.0529 0.172 Uiso 1 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N6 172.5(2) . . ?
N1 Cu1 O1 89.05(19) . . ?
N6 Cu1 O1 87.39(18) . . ?
N1 Cu1 Cl1 93.03(17) . . ?
N6 Cu1 Cl1 91.70(16) . . ?
O1 Cu1 Cl1 169.16(14) . . ?
N3 Cu2 N2 174.4(2) . . ?
N3 Cu2 O1 87.94(19) . . ?
N2 Cu2 O1 88.19(19) . . ?
N3 Cu2 Cl2 91.02(16) . . ?
N2 Cu2 Cl2 93.63(17) . . ?
O1 Cu2 Cl2 167.57(13) . . ?
N5 Cu3 N4 160.0(2) . . ?
N5 Cu3 O1 88.10(18) . . ?
N4 Cu3 O1 89.02(19) . . ?
N5 Cu3 N7 91.2(2) . . ?
N4 Cu3 N7 94.6(2) . . ?
O1 Cu3 N7 170.90(19) . . ?
N5 Cu3 Cl3 105.30(16) . . ?
N4 Cu3 Cl3 93.51(16) . . ?
O1 Cu3 Cl3 78.36(12) . . ?
N7 Cu3 Cl3 93.09(16) . . ?
Cu2 O1 Cu1 116.35(19) . . ?
Cu2 O1 Cu3 107.99(18) . . ?
Cu1 O1 Cu3 108.90(18) . . ?
C3 N1 N2 107.2(5) . . ?
C3 N1 Cu1 130.8(5) . . ?
N2 N1 Cu1 122.0(4) . . ?
N1 N2 C1 107.5(6) . . ?
N1 N2 Cu2 122.4(4) . . ?
C1 N2 Cu2 130.0(5) . . ?
C6 N3 N4 106.8(6) . . ?
C6 N3 Cu2 134.3(5) . . ?
N4 N3 Cu2 118.9(4) . . ?
C4 N4 N3 108.1(5) . . ?
C4 N4 Cu3 132.5(5) . . ?
N3 N4 Cu3 118.8(4) . . ?
C9 N5 N6 107.0(5) . . ?
C9 N5 Cu3 133.6(5) . . ?
N6 N5 Cu3 119.3(3) . . ?
C7 N6 N5 107.8(5) . . ?
C7 N6 Cu1 133.0(5) . . ?
N5 N6 Cu1 119.2(4) . . ?
C12 N7 N8 104.6(5) . . ?
C12 N7 Cu3 134.7(5) . . ?
N8 N7 Cu3 120.1(4) . . ?
C10 N8 N7 111.5(5) . . ?
C15 N9 C17 114.2(7) . . ?
C15 N9 C13 116.0(7) . . ?
C17 N9 C13 109.3(6) . . ?
N2 C1 C2 110.4(7) . . ?
C1 C2 C3 103.9(6) . . ?
N1 C3 C2 111.0(7) . . ?
N4 C4 C5 109.8(7) . . ?
C6 C5 C4 105.4(7) . . ?
C5 C6 N3 110.0(7) . . ?
N6 C7 C8 109.6(6) . . ?
C9 C8 C7 105.6(6) . . ?
N5 C9 C8 110.1(6) . . ?
N8 C10 C11 107.4(6) . . ?
C10 C11 C12 105.9(6) . . ?
N7 C12 C11 110.5(7) . . ?
N9 C13 C14 112.5(7) . . ?
N9 C15 C16 112.5(8) . . ?
C18 C17 N9 117.0(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 1.929(5) . ?
Cu1 N6 1.945(5) . ?
Cu1 O1 2.012(4) . ?
Cu1 Cl1 2.257(2) . ?
Cu2 N3 1.932(5) . ?
Cu2 N2 1.949(5) . ?
Cu2 O1 2.006(4) . ?
Cu2 Cl2 2.3158(19) . ?
Cu3 N5 1.937(5) . ?
Cu3 N4 1.950(5) . ?
Cu3 O1 2.016(4) . ?
Cu3 N7 2.016(5) . ?
Cu3 Cl3 2.6763(18) . ?
N1 C3 1.340(8) . ?
N1 N2 1.345(7) . ?
N2 C1 1.350(8) . ?
N3 C6 1.355(8) . ?
N3 N4 1.363(7) . ?
N4 C4 1.331(8) . ?
N5 C9 1.338(7) . ?
N5 N6 1.377(7) . ?
N6 C7 1.335(8) . ?
N7 C12 1.335(8) . ?
N7 N8 1.351(7) . ?
N8 C10 1.329(8) . ?
N9 C15 1.486(10) . ?
N9 C17 1.496(10) . ?
N9 C13 1.503(10) . ?
C1 C2 1.363(10) . ?
C2 C3 1.366(10) . ?
C4 C5 1.371(10) . ?
C5 C6 1.354(10) . ?
C7 C8 1.368(9) . ?
C8 C9 1.364(9) . ?
C10 C11 1.350(10) . ?
C11 C12 1.378(10) . ?
C13 C14 1.516(11) . ?
C15 C16 1.519(12) . ?
C17 C18 1.478(12) . ?
