#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:55:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179431 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/28/4332869.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_4332869
loop_
_publ_author_name
'Lang, Jian-Ping'
'Xu, Qing-Feng'
'Zhang, Wen-Hua'
'Li, Hong-Xi'
'Ren, Zhi-Gang'
'Chen, Jin-Xiang'
'Zhang, Yong'
_publ_section_title
;
 Mo(W)/Cu/S Cluster-Based Supramolecular Arrays Assembled from Preformed
 Clusters [Et4N]4[WS4Cu4I6] and [(n-Bu)4N]2[MoOS3Cu3X3] (X = I, SCN) with
 Flexible Ditopic Ligands
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10487
_journal_page_last               10496
_journal_paper_doi               10.1021/ic060974d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C17 H12 Cu3 Mo N6 O S3, C3 H7 N O, C2 H3 N'
_chemical_formula_sum            'C22 H22 Cu3 Mo N8 O2 S3'
_chemical_formula_weight         813.22
_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                95.68(3)
_cell_angle_beta                 94.28(3)
_cell_angle_gamma                114.64(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2794(19)
_cell_length_b                   11.063(2)
_cell_length_c                   15.852(3)
_cell_measurement_reflns_used    5089
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1459.8(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16615
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.826
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.6018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0718
_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)+(0.0403P)²+7.7090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                5383
_reflns_number_total             6574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060974dsup4.cif
_cod_data_source_block           tmp
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332869
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
Mo1 Mo 0.51500(6) 0.87424(5) 0.59005(3) 0.02013(14) Uani 1 1 d .
Cu1 Cu 0.38152(9) 0.82482(8) 0.73575(5) 0.0259(2) Uani 1 1 d .
Cu2 Cu 0.75665(10) 0.83624(8) 0.66384(5) 0.0259(2) Uani 1 1 d .
Cu3 Cu 0.65930(10) 1.12944(8) 0.65539(6) 0.0296(2) Uani 1 1 d .
S1 S 0.40081(19) 0.99344(16) 0.65995(11) 0.0255(4) Uani 1 1 d .
S2 S 0.4927(2) 0.70343(16) 0.66287(11) 0.0273(4) Uani 1 1 d .
S3 S 0.77871(18) 1.01071(16) 0.59311(11) 0.0255(4) Uani 1 1 d .
O1 O 0.4250(5) 0.8153(5) 0.4860(3) 0.0287(10) Uani 1 1 d .
O2 O 0.4097(14) 0.3789(14) -0.1571(7) 0.149(5) Uani 1 1 d D
N1 N 0.5209(7) 0.9044(6) 0.8556(4) 0.0296(13) Uani 1 1 d .
N2 N 0.1702(7) 0.7053(6) 0.7640(4) 0.0328(14) Uani 1 1 d .
N3 N 0.9088(7) 0.8932(6) 0.7738(4) 0.0308(13) Uani 1 1 d .
N4 N 0.8440(6) 0.7154(5) 0.5974(4) 0.0265(12) Uani 1 1 d .
N5 N 0.7706(7) 1.3049(6) 0.7169(4) 0.0350(14) Uani 1 1 d .
N6 N 0.9127(8) 1.5354(6) 0.7898(5) 0.0499(19) Uani 1 1 d .
N7 N 0.3106(9) 0.3379(8) -0.2947(6) 0.056(2) Uani 1 1 d .
N8 N 0.857(3) 0.650(3) 0.0569(16) 0.224(9) Uiso 1 1 d D
C1 C 0.5110(10) 0.8258(9) 0.9146(5) 0.049(2) Uani 1 1 d .
H1 H 0.4262 0.7379 0.9056 0.059 Uiso 1 1 calc R
C2 C 0.6163(10) 0.8642(9) 0.9883(5) 0.047(2) Uani 1 1 d .
H2 H 0.6023 0.8034 1.0286 0.056 Uiso 1 1 calc R
C3 C 0.7406(9) 0.9888(8) 1.0040(4) 0.0325(16) Uani 1 1 d .
C4 C 0.7517(11) 1.0731(8) 0.9434(5) 0.050(2) Uani 1 1 d .
H4 H 0.8345 1.1619 0.9518 0.060 Uiso 1 1 calc R
C5 C 0.6425(11) 1.0276(8) 0.8711(5) 0.049(2) Uani 1 1 d .
H5 H 0.6534 1.0865 0.8298 0.059 Uiso 1 1 calc R
C6 C 0.8618(8) 1.0318(7) 1.0810(4) 0.0304(15) Uani 1 1 d .
C7 C 0.8305(11) 0.9646(10) 1.1508(6) 0.062(3) Uani 1 1 d .
H7 H 0.7298 0.8907 1.1505 0.074 Uiso 1 1 calc R
C8 C 0.0512(8) 0.6207(7) 0.7736(4) 0.0285(15) Uani 1 1 d .
C9 C 0.8823(9) 0.8257(8) 0.8394(5) 0.0352(17) Uani 1 1 d .
H9 H 0.7826 0.7498 0.8368 0.042 Uiso 1 1 calc R
C10 C 0.9914(9) 0.8593(8) 0.9119(5) 0.0374(17) Uani 1 1 d .
H10 H 0.9649 0.8069 0.9572 0.045 Uiso 1 1 calc R
C11 C 1.0549(11) 0.9957(10) 0.7784(6) 0.060(3) Uani 1 1 d .
H11 H 1.0805 1.0430 0.7307 0.072 Uiso 1 1 calc R
C12 C 0.7673(10) 0.5807(7) 0.5910(5) 0.0398(18) Uani 1 1 d .
H12 H 0.6688 0.5433 0.6138 0.048 Uiso 1 1 calc R
C13 C 0.8224(9) 0.4944(7) 0.5535(5) 0.0371(18) Uani 1 1 d .
H13 H 0.7622 0.4001 0.5503 0.045 Uiso 1 1 calc R
C14 C 0.9683(8) 0.5457(6) 0.5199(4) 0.0231(13) Uani 1 1 d .
C15 C 1.0447(8) 0.6838(7) 0.5243(5) 0.0341(17) Uani 1 1 d .
H15 H 1.1419 0.7238 0.5005 0.041 Uiso 1 1 calc R
C16 C 0.9807(8) 0.7637(7) 0.5629(5) 0.0321(16) Uani 1 1 d .
H16 H 1.0367 0.8583 0.5652 0.039 Uiso 1 1 calc R
C17 C 0.8429(8) 1.4125(7) 0.7498(5) 0.0319(16) Uani 1 1 d .
C18 C 0.1757(14) 0.3623(13) -0.2815(10) 0.097(5) Uani 1 1 d .
H18A H 0.1732 0.3812 -0.2201 0.145 Uiso 1 1 calc R
H18B H 0.0783 0.2830 -0.3065 0.145 Uiso 1 1 calc R
H18C H 0.1820 0.4398 -0.3089 0.145 Uiso 1 1 calc R
C19 C 0.3270(15) 0.3002(11) -0.3819(7) 0.075(3) Uani 1 1 d .
H19A H 0.3476 0.3764 -0.4135 0.113 Uiso 1 1 calc R
H19B H 0.2282 0.2238 -0.4087 0.113 Uiso 1 1 calc R
H19C H 0.4163 0.2749 -0.3828 0.113 Uiso 1 1 calc R
C20 C 0.4201(15) 0.3521(15) -0.2326(9) 0.088(4) Uani 1 1 d .
H20 H 0.5120 0.3411 -0.2468 0.106 Uiso 1 1 calc R
C21 C 0.723(4) 0.436(4) -0.032(3) 0.48(4) Uiso 1 1 d D
H21A H 0.7673 0.3774 -0.0585 0.726 Uiso 1 1 calc R
H21B H 0.6695 0.4641 -0.0761 0.726 Uiso 1 1 calc R
H21C H 0.6449 0.3859 0.0052 0.726 Uiso 1 1 calc R
C22 C 0.850(4) 0.552(4) 0.019(4) 0.43(3) Uiso 1 1 d 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'
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'
S S 0.1246 0.1234 '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'
Mo Mo -1.6832 0.6857 '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 Mo1 S2 111.13(16) . .
O1 Mo1 S1 111.07(16) . .
S2 Mo1 S1 107.64(7) . .
O1 Mo1 S3 110.39(16) . .
S2 Mo1 S3 108.41(7) . .
S1 Mo1 S3 108.07(7) . .
O1 Mo1 Cu3 124.48(16) . .
S2 Mo1 Cu3 124.39(6) . .
S1 Mo1 Cu3 54.13(5) . .
S3 Mo1 Cu3 54.02(5) . .
O1 Mo1 Cu2 126.27(16) . .
S2 Mo1 Cu2 54.24(5) . .
S1 Mo1 Cu2 122.66(6) . .
S3 Mo1 Cu2 54.18(5) . .
Cu3 Mo1 Cu2 89.60(4) . .
O1 Mo1 Cu1 128.49(15) . .
S2 Mo1 Cu1 54.09(5) . .
S1 Mo1 Cu1 53.56(5) . .
S3 Mo1 Cu1 121.12(6) . .
Cu3 Mo1 Cu1 88.15(4) . .
Cu2 Mo1 Cu1 87.37(4) . .
N2 Cu1 N1 103.6(2) . .
N2 Cu1 S1 118.81(19) . .
N1 Cu1 S1 110.08(17) . .
N2 Cu1 S2 110.65(18) . .
N1 Cu1 S2 106.68(17) . .
S1 Cu1 S2 106.48(7) . .
N2 Cu1 Mo1 135.06(18) . .
N1 Cu1 Mo1 120.88(16) . .
S1 Cu1 Mo1 53.46(5) . .
S2 Cu1 Mo1 53.03(5) . .
N3 Cu2 N4 99.0(2) . .
N3 Cu2 S2 120.45(18) . .
N4 Cu2 S2 105.02(16) . .
N3 Cu2 S3 113.19(18) . .
N4 Cu2 S3 110.30(16) . .
S2 Cu2 S3 107.96(7) . .
N3 Cu2 Mo1 141.00(17) . .
N4 Cu2 Mo1 119.99(16) . .
S2 Cu2 Mo1 53.79(5) . .
S3 Cu2 Mo1 54.18(5) . .
N5 Cu3 S3 124.10(19) . .
N5 Cu3 S1 124.90(19) . .
S3 Cu3 S1 109.55(7) . .
N5 Cu3 Mo1 171.8(2) . .
S3 Cu3 Mo1 54.88(5) . .
S1 Cu3 Mo1 54.76(5) . .
Cu3 S1 Mo1 71.11(6) . .
Cu3 S1 Cu1 110.08(8) . .
Mo1 S1 Cu1 72.98(6) . .
Mo1 S2 Cu2 71.97(6) . .
Mo1 S2 Cu1 72.88(6) . .
Cu2 S2 Cu1 108.61(8) . .
Cu3 S3 Mo1 71.09(6) . .
Cu3 S3 Cu2 111.02(8) . .
Mo1 S3 Cu2 71.64(6) . .
C1 N1 C5 116.0(7) . .
C1 N1 Cu1 120.3(5) . .
C5 N1 Cu1 122.6(5) . .
C8 N2 Cu1 169.6(6) . .
C9 N3 C11 116.1(6) . .
C9 N3 Cu2 123.8(5) . .
C11 N3 Cu2 119.6(5) . .
C16 N4 C12 116.1(6) . .
C16 N4 Cu2 123.5(4) . .
C12 N4 Cu2 120.3(5) . .
C17 N5 Cu3 175.8(7) . .
C8 N6 C17 121.8(7) 1_665 .
C20 N7 C18 123.1(11) . .
C20 N7 C19 120.3(9) . .
C18 N7 C19 116.6(10) . .
N1 C1 C2 123.6(8) . .
N1 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
C3 C2 C1 120.5(8) . .
C3 C2 H2 119.7 . .
C1 C2 H2 119.7 . .
C2 C3 C4 116.6(7) . .
C2 C3 C6 122.2(7) . .
C4 C3 C6 121.2(7) . .
C5 C4 C3 119.6(8) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
N1 C5 C4 123.6(8) . .
N1 C5 H5 118.2 . .
C4 C5 H5 118.2 . .
C7 C6 C10 116.0(7) . 2_777
C7 C6 C3 120.7(7) . .
C10 C6 C3 123.3(7) 2_777 .
C6 C7 C11 120.3(8) . 2_777
C6 C7 H7 119.9 . .
C11 C7 H7 119.9 2_777 .
N2 C8 N6 173.2(7) . 1_445
N3 C9 C10 123.7(7) . .
N3 C9 H9 118.2 . .
C10 C9 H9 118.2 . .
C6 C10 C9 120.7(7) 2_777 .
C6 C10 H10 119.7 2_777 .
C9 C10 H10 119.7 . .
N3 C11 C7 123.2(8) . 2_777
N3 C11 H11 118.4 . .
C7 C11 H11 118.4 2_777 .
N4 C12 C13 124.0(7) . .
N4 C12 H12 118.0 . .
C13 C12 H12 118.0 . .
C12 C13 C14 119.7(6) . .
C12 C13 H13 120.2 . .
C14 C13 H13 120.2 . .
C15 C14 C13 116.3(6) . .
C15 C14 C14 123.0(7) . 2_766
C13 C14 C14 120.7(7) . 2_766
C16 C15 C14 120.4(6) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
N4 C16 C15 123.6(6) . .
N4 C16 H16 118.2 . .
C15 C16 H16 118.2 . .
N5 C17 N6 174.4(8) . .
N7 C18 H18A 109.5 . .
N7 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
N7 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N7 C19 H19A 109.5 . .
N7 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
N7 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O2 C20 N7 123.2(12) . .
O2 C20 H20 118.4 . .
N7 C20 H20 118.4 . .
C22 C21 H21A 109.5 . .
C22 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C22 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
N8 C22 C21 134(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.724(5) .
Mo1 S2 2.2555(18) .
Mo1 S1 2.2672(18) .
Mo1 S3 2.2710(18) .
Mo1 Cu3 2.6265(14) .
Mo1 Cu2 2.6582(12) .
Mo1 Cu1 2.6981(12) .
Cu1 N2 1.970(6) .
Cu1 N1 2.100(6) .
Cu1 S1 2.2701(19) .
Cu1 S2 2.2867(19) .
Cu2 N3 2.025(6) .
Cu2 N4 2.075(6) .
Cu2 S2 2.269(2) .
Cu2 S3 2.2711(19) .
Cu3 N5 1.894(6) .
Cu3 S3 2.2467(19) .
Cu3 S1 2.250(2) .
O2 C20 1.225(14) .
N1 C1 1.322(10) .
N1 C5 1.342(10) .
N2 C8 1.145(8) .
N3 C9 1.319(9) .
N3 C11 1.347(10) .
N4 C16 1.338(9) .
N4 C12 1.347(9) .
N5 C17 1.140(9) .
N6 C8 1.301(9) 1_665
N6 C17 1.305(9) .
N7 C20 1.309(14) .
N7 C18 1.412(12) .
N7 C19 1.442(13) .
N8 C22 1.16(6) .
C1 C2 1.372(11) .
C1 H1 0.9500 .
C2 C3 1.363(11) .
C2 H2 0.9500 .
C3 C4 1.384(11) .
C3 C6 1.487(9) .
C4 C5 1.371(11) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.376(11) .
C6 C10 1.379(10) 2_777
C7 C11 1.386(11) 2_777
C7 H7 0.9500 .
C8 N6 1.301(9) 1_445
C9 C10 1.382(10) .
C9 H9 0.9500 .
C10 C6 1.379(10) 2_777
C10 H10 0.9500 .
C11 C7 1.386(11) 2_777
C11 H11 0.9500 .
C12 C13 1.365(10) .
C12 H12 0.9500 .
C13 C14 1.402(9) .
C13 H13 0.9500 .
C14 C15 1.382(9) .
C14 C14 1.481(12) 2_766
C15 C16 1.376(9) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20 0.9500 .
C21 C22 1.44(7) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
