#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:48:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179425 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/22/4332253.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332253
loop_
_publ_author_name
'Zhang, Qian-Feng'
'Yu, Zhan'
'Ding, Jihai'
'Song, Yinglin'
'Rothenberger, Alexander'
'Fenske, Dieter'
'Leung, Wa-Hung'
_publ_section_title
;
 Construction of New Heteroselenometallic Clusters:  Formation of
 Crownlike [Et4N]4[(μ5-WSe4)(CuI)5(μ-I)2] and Octahedral Polymeric
 [(μ6-WSe4)Cu6I4(py)4]nfrom Planar [Et4N]4[(μ4-WSe4)Cu4I6] with
 Additional Faces
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5187
_journal_page_last               5195
_journal_paper_doi               10.1021/ic060161p
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C15 H15 Cu3 I N3 O Se3 W'
_chemical_formula_weight         991.55
_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                102.88(3)
_cell_angle_beta                 97.93(3)
_cell_angle_gamma                94.94(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2156(16)
_cell_length_b                   8.8229(18)
_cell_length_c                   15.840(3)
_cell_measurement_reflns_used    1467
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      54.47
_cell_measurement_theta_min      5.22
_cell_volume                     1100.4(4)
_computing_cell_refinement       'stoe winexpose'
_computing_data_collection       'stoe winexpose'
_computing_data_reduction        'stoe winexpose'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'stoe stad'
_diffrn_measurement_method       'area deector'
_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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7479
_diffrn_reflns_theta_full        26.94
_diffrn_reflns_theta_max         26.94
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    14.444
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0581
_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)+(0.1592P)²+3.0975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                3917
_reflns_number_total             4414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060161psup1.cif
_cod_data_source_block           q27a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1100.5(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332253
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
W1 W 0.06855(5) -0.16738(5) 0.83071(3) 0.0266(2) Uani 1 1 d .
Se1 Se 0.03444(14) -0.21993(13) 0.67444(7) 0.0286(3) Uani 1 1 d .
Se2 Se -0.12249(15) 0.01032(13) 0.88590(8) 0.0289(3) Uani 1 1 d .
Se3 Se 0.34666(15) -0.05100(14) 0.89200(8) 0.0308(3) Uani 1 1 d .
Cu1 Cu -0.16439(18) -0.05379(16) 0.72785(10) 0.0299(3) Uani 1 1 d .
Cu2 Cu 0.30753(18) -0.07874(16) 0.73558(10) 0.0297(3) Uani 1 1 d .
Cu3 Cu 0.15368(19) 0.11322(17) 0.94738(10) 0.0336(4) Uani 1 1 d .
I1 I -0.46181(9) -0.22866(8) 0.66888(5) 0.0289(2) Uani 1 1 d .
O1 O 0.0294(9) -0.3533(10) 0.8612(5) 0.0280(16) Uani 1 1 d .
N10 N -0.1847(12) 0.1303(11) 0.6717(7) 0.029(2) Uani 1 1 d .
N20 N 0.3085(12) 0.1297(11) 0.6944(7) 0.029(2) Uani 1 1 d .
N30 N 0.2426(13) 0.3242(11) 1.0137(6) 0.031(2) Uani 1 1 d .
C11 C -0.1822(18) 0.1143(15) 0.5856(8) 0.038(3) Uani 1 1 d .
H11 H -0.1645 0.0178 0.5524 0.045 Uiso 1 1 calc R
C12 C -0.2052(17) 0.2365(17) 0.5435(9) 0.040(3) Uani 1 1 d .
H12 H -0.2037 0.2217 0.4837 0.048 Uiso 1 1 calc R
C13 C -0.2300(16) 0.3792(15) 0.5933(9) 0.036(3) Uani 1 1 d .
H13 H -0.2456 0.4628 0.5674 0.043 Uiso 1 1 calc R
C14 C -0.2317(18) 0.3971(15) 0.6821(10) 0.041(3) Uani 1 1 d .
H14 H -0.2483 0.4927 0.7166 0.049 Uiso 1 1 calc R
C15 C -0.2082(16) 0.2711(14) 0.7189(7) 0.032(2) Uani 1 1 d .
H15 H -0.2088 0.2842 0.7787 0.038 Uiso 1 1 calc R
C21 C 0.3628(16) 0.1465(14) 0.6214(9) 0.036(3) Uani 1 1 d .
H21 H 0.4211 0.0693 0.5939 0.043 Uiso 1 1 calc R
C22 C 0.3385(17) 0.2698(15) 0.5840(9) 0.039(3) Uani 1 1 d .
H22 H 0.3789 0.2752 0.5325 0.047 Uiso 1 1 calc R
C23 C 0.2537(17) 0.3853(15) 0.6234(10) 0.041(3) Uani 1 1 d .
H23 H 0.2362 0.4710 0.5996 0.049 Uiso 1 1 calc R
C24 C 0.1947(15) 0.3721(13) 0.6992(9) 0.036(3) Uani 1 1 d .
H24 H 0.1370 0.4492 0.7274 0.043 Uiso 1 1 calc R
C25 C 0.2230(16) 0.2404(14) 0.7336(9) 0.036(3) Uani 1 1 d .
H25 H 0.1817 0.2302 0.7841 0.043 Uiso 1 1 calc R
C31 C 0.2053(18) 0.4509(14) 0.9826(9) 0.038(3) Uani 1 1 d .
H31 H 0.1231 0.4386 0.9342 0.045 Uiso 1 1 calc R
C32 C 0.2895(17) 0.5997(16) 1.0230(9) 0.040(3) Uani 1 1 d .
H32 H 0.2672 0.6842 0.9990 0.048 Uiso 1 1 calc R
C33 C 0.4044(17) 0.6221(14) 1.0973(9) 0.038(3) Uani 1 1 d .
H33 H 0.4610 0.7206 1.1245 0.046 Uiso 1 1 calc R
C34 C 0.4328(16) 0.4940(15) 1.1301(10) 0.039(3) Uani 1 1 d .
H34 H 0.5057 0.5064 1.1823 0.047 Uiso 1 1 calc R
C35 C 0.3553(16) 0.3475(16) 1.0871(10) 0.041(3) Uani 1 1 d .
H35 H 0.3814 0.2619 1.1092 0.049 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'
I I -0.4742 1.8119 '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
O1 W1 Se1 108.0(2) . .
O1 W1 Se3 109.5(2) . .
Se1 W1 Se3 109.58(5) . .
O1 W1 Se2 110.2(2) . .
Se1 W1 Se2 110.47(5) . .
Se3 W1 Se2 109.08(5) . .
O1 W1 Cu3 124.2(2) . .
Se1 W1 Cu3 127.81(5) . .
Se3 W1 Cu3 54.76(5) . .
Se2 W1 Cu3 54.35(5) . .
O1 W1 Cu1 122.7(2) . .
Se1 W1 Cu1 55.35(4) . .
Se3 W1 Cu1 127.75(5) . .
Se2 W1 Cu1 55.18(4) . .
Cu3 W1 Cu1 93.00(5) . .
O1 W1 Cu2 128.5(2) . .
Se1 W1 Cu2 55.25(5) . .
Se3 W1 Cu2 54.59(5) . .
Se2 W1 Cu2 121.31(4) . .
Cu3 W1 Cu2 88.39(5) . .
Cu1 W1 Cu2 89.22(5) . .
W1 Se1 Cu1 69.85(5) . .
W1 Se1 Cu2 70.95(6) . .
Cu1 Se1 Cu2 107.16(7) . .
Cu3 Se2 Cu1 112.08(7) . .
Cu3 Se2 W1 68.99(5) . .
Cu1 Se2 W1 69.13(5) . .
Cu3 Se3 W1 69.30(6) . .
Cu3 Se3 Cu2 107.01(7) . .
W1 Se3 Cu2 71.11(6) . .
N10 Cu1 Se1 113.7(3) . .
N10 Cu1 Se2 115.5(3) . .
Se1 Cu1 Se2 110.43(7) . .
N10 Cu1 I1 103.1(3) . .
Se1 Cu1 I1 105.19(6) . .
Se2 Cu1 I1 108.09(7) . .
N10 Cu1 W1 139.0(3) . .
Se1 Cu1 W1 54.79(4) . .
Se2 Cu1 W1 55.70(4) . .
I1 Cu1 W1 117.85(6) . .
N20 Cu2 Se3 115.6(3) . .
N20 Cu2 Se1 105.0(3) . .
Se3 Cu2 Se1 107.85(7) . .
N20 Cu2 I1 107.3(3) . 1_655
Se3 Cu2 I1 109.98(6) . 1_655
Se1 Cu2 I1 111.11(6) . 1_655
N20 Cu2 W1 121.4(3) . .
Se3 Cu2 W1 54.30(5) . .
Se1 Cu2 W1 53.80(4) . .
I1 Cu2 W1 131.06(6) 1_655 .
N30 Cu3 Se2 129.3(3) . .
N30 Cu3 Se3 116.6(3) . .
Se2 Cu3 Se3 112.56(7) . .
N30 Cu3 W1 168.2(3) . .
Se2 Cu3 W1 56.65(5) . .
Se3 Cu3 W1 55.94(5) . .
Cu2 I1 Cu1 109.71(6) 1_455 .
C11 N10 C15 117.8(9) . .
C11 N10 Cu1 121.3(8) . .
C15 N10 Cu1 120.9(8) . .
C21 N20 C25 117.9(10) . .
C21 N20 Cu2 122.7(7) . .
C25 N20 Cu2 118.2(8) . .
C35 N30 C31 118.2(11) . .
C35 N30 Cu3 120.7(8) . .
C31 N30 Cu3 120.8(9) . .
N10 C11 C12 122.9(11) . .
C13 C12 C11 118.2(12) . .
C12 C13 C14 119.4(11) . .
C15 C14 C13 119.2(11) . .
N10 C15 C14 122.7(11) . .
N20 C21 C22 124.3(11) . .
C21 C22 C23 118.9(12) . .
C22 C23 C24 118.7(11) . .
C23 C24 C25 119.3(11) . .
N20 C25 C24 121.0(12) . .
N30 C31 C32 120.6(12) . .
C33 C32 C31 120.7(12) . .
C32 C33 C34 117.4(13) . .
C33 C34 C35 121.0(13) . .
N30 C35 C34 121.9(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.826(9) .
W1 Se1 2.3865(13) .
W1 Se3 2.3993(16) .
W1 Se2 2.4243(13) .
W1 Cu3 2.7091(19) .
W1 Cu1 2.7421(17) .
W1 Cu2 2.7953(16) .
Se1 Cu1 2.4030(17) .
Se1 Cu2 2.430(2) .
Se2 Cu3 2.358(2) .
Se2 Cu1 2.4091(18) .
Se3 Cu3 2.3655(18) .
Se3 Cu2 2.4081(19) .
Cu1 N10 2.026(9) .
Cu1 I1 2.702(2) .
Cu2 N20 2.084(9) .
Cu2 I1 2.6112(16) 1_655
Cu3 N30 1.945(10) .
I1 Cu2 2.6112(16) 1_455
N10 C11 1.343(15) .
N10 C15 1.344(15) .
N20 C21 1.329(15) .
N20 C25 1.342(14) .
N30 C35 1.346(18) .
N30 C31 1.360(14) .
C11 C12 1.401(17) .
C12 C13 1.376(19) .
C13 C14 1.382(19) .
C14 C15 1.381(16) .
C21 C22 1.366(17) .
C22 C23 1.368(18) .
C23 C24 1.38(2) .
C24 C25 1.412(16) .
C31 C32 1.40(2) .
C32 C33 1.37(2) .
C33 C34 1.369(18) .
C34 C35 1.37(2) .
