#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:12:01 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179561 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/30/4503078.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_4503078
loop_
_publ_author_name
'Zhang, Wen-Hua'
'Song, Ying-Lin'
'Zhang, Yong'
'Lang, Jian-Ping'
_publ_section_title
;
 Binuclear Cluster-to-Cluster-Based Supramolecular Compounds: Design,
 Assembly, and Enhanced Third-Order Nonlinear Optical Performances of
 {[Et4N]2[MoOS3Cu2(μ-CN)]2·2aniline}nand
 {[Et4N]4[MoOS3Cu3CN(μ′-CN)]2(μ-CN)2}n
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              253
_journal_paper_doi               10.1021/cg070235n
_journal_volume                  8
_journal_year                    2008
_chemical_formula_moiety         'C Cu2 Mo N O S3, C8 H20 N, C6 H7 N'
_chemical_formula_sum            'C15 H27 Cu2 Mo N3 O S3'
_chemical_formula_weight         584.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.908(3)
_cell_length_b                   16.105(3)
_cell_length_c                   11.332(2)
_cell_measurement_reflns_used    6972
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2119.5(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_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      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23654
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.876
_exptl_absorpt_correction_T_max  0.7819
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0515
_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)+(0.0171P)²+5.1859P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0861
_reflns_number_gt                3795
_reflns_number_total             4854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg070235n-file003.cif
_cod_data_source_block           tmp
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4503078
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.18377(3) 0.49670(2) 0.67755(3) 0.01835(10) Uani 1 1 d .
Cu1 Cu 0.03591(5) 0.62372(3) 0.64016(6) 0.02605(15) Uani 1 1 d .
Cu2 Cu 0.01893(5) 0.38234(3) 0.64572(6) 0.02529(15) Uani 1 1 d .
S1 S 0.16731(10) 0.60746(7) 0.55498(12) 0.0233(2) Uani 1 1 d .
S2 S 0.05170(9) 0.50506(7) 0.75765(10) 0.0216(2) Uani 1 1 d .
S3 S 0.15380(10) 0.37882(7) 0.56279(11) 0.0217(2) Uani 1 1 d .
O1 O 0.3194(3) 0.4944(2) 0.8054(3) 0.0335(8) Uani 1 1 d .
N1 N 0.0207(3) 0.7266(3) 0.7211(4) 0.0300(9) Uani 1 1 d .
N2 N -0.2885(3) 0.6103(2) 0.8179(4) 0.0223(8) Uani 1 1 d .
N3 N 0.4644(5) 0.6057(4) 1.0358(6) 0.0525(13) Uani 1 1 d D
C1 C 0.0084(4) 0.7849(2) 0.7718(4) 0.0176(9) Uani 1 1 d .
C2 C -0.3865(4) 0.6624(3) 0.7233(5) 0.0322(12) Uani 1 1 d .
H2A H -0.3784 0.6676 0.6406 0.039 Uiso 1 1 calc R
H2B H -0.3800 0.7188 0.7606 0.039 Uiso 1 1 calc R
C3 C -0.5067(5) 0.6284(4) 0.6910(6) 0.0486(16) Uani 1 1 d .
H3A H -0.5163 0.6237 0.7718 0.073 Uiso 1 1 calc R
H3B H -0.5155 0.5735 0.6504 0.073 Uiso 1 1 calc R
H3C H -0.5651 0.6661 0.6301 0.073 Uiso 1 1 calc R
C4 C -0.2919(5) 0.5238(3) 0.7649(5) 0.0324(12) Uani 1 1 d .
H4A H -0.3607 0.4950 0.7619 0.039 Uiso 1 1 calc R
H4B H -0.2234 0.4931 0.8273 0.039 Uiso 1 1 calc R
C5 C -0.2946(5) 0.5185(4) 0.6295(5) 0.0461(15) Uani 1 1 d .
H5A H -0.2292 0.5492 0.6294 0.069 Uiso 1 1 calc R
H5B H -0.3666 0.5428 0.5646 0.069 Uiso 1 1 calc R
H5C H -0.2900 0.4603 0.6075 0.069 Uiso 1 1 calc R
C6 C -0.2943(4) 0.6011(3) 0.9477(4) 0.0268(10) Uani 1 1 d .
H6A H -0.2289 0.5661 1.0062 0.032 Uiso 1 1 calc R
H6B H -0.3661 0.5712 0.9324 0.032 Uiso 1 1 calc R
C7 C -0.2912(4) 0.6818(3) 1.0180(5) 0.0340(12) Uani 1 1 d .
H7A H -0.3596 0.7149 0.9649 0.051 Uiso 1 1 calc R
H7B H -0.2218 0.7130 1.0313 0.051 Uiso 1 1 calc R
H7C H -0.2904 0.6697 1.1032 0.051 Uiso 1 1 calc R
C8 C -0.1783(4) 0.6548(3) 0.8367(5) 0.0274(10) Uani 1 1 d .
H8A H -0.1732 0.6547 0.7520 0.033 Uiso 1 1 calc R
H8B H -0.1836 0.7134 0.8599 0.033 Uiso 1 1 calc R
C9 C -0.0688(4) 0.6181(4) 0.9403(5) 0.0362(12) Uani 1 1 d .
H9A H -0.0655 0.5588 0.9227 0.054 Uiso 1 1 calc R
H9B H -0.0676 0.6252 1.0268 0.054 Uiso 1 1 calc R
H9C H -0.0023 0.6464 0.9386 0.054 Uiso 1 1 calc R
C10 C 0.4171(5) 0.6346(3) 1.1136(6) 0.0363(12) Uani 1 1 d .
C11 C 0.3014(5) 0.6579(3) 1.0611(6) 0.0419(14) Uani 1 1 d .
H11 H 0.2540 0.6524 0.9697 0.050 Uiso 1 1 calc R
C12 C 0.2562(5) 0.6887(3) 1.1411(7) 0.0477(15) Uani 1 1 d .
H12 H 0.1773 0.7041 1.1036 0.057 Uiso 1 1 calc R
C13 C 0.3213(6) 0.6982(4) 1.2741(7) 0.0548(17) Uani 1 1 d .
H13 H 0.2886 0.7195 1.3285 0.066 Uiso 1 1 calc R
C14 C 0.4355(5) 0.6756(4) 1.3254(6) 0.0468(15) Uani 1 1 d .
H14 H 0.4823 0.6821 1.4168 0.056 Uiso 1 1 calc R
C15 C 0.4839(5) 0.6439(3) 1.2485(6) 0.0410(14) Uani 1 1 d .
H15 H 0.5628 0.6283 1.2870 0.049 Uiso 1 1 calc R
H16 H 0.526(4) 0.573(4) 1.073(7) 0.09(3) Uiso 1 1 d D
H17 H 0.416(5) 0.584(5) 0.960(4) 0.09(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 S1 109.26(13) . .
O1 Mo1 S3 109.01(12) . .
S1 Mo1 S3 111.97(5) . .
O1 Mo1 S2 109.44(12) . .
S1 Mo1 S2 108.77(4) . .
S3 Mo1 S2 108.36(4) . .
O1 Mo1 Cu1 122.60(12) . .
S1 Mo1 Cu1 54.81(4) . .
S3 Mo1 Cu1 128.33(4) . .
S2 Mo1 Cu1 54.01(3) . .
O1 Mo1 Cu2 123.25(12) . .
S1 Mo1 Cu2 127.45(4) . .
S3 Mo1 Cu2 54.61(3) . .
S2 Mo1 Cu2 53.76(3) . .
Cu1 Mo1 Cu2 91.94(3) . .
N1 Cu1 S2 116.04(12) . .
N1 Cu1 S1 122.61(12) . .
S2 Cu1 S1 104.72(5) . .
N1 Cu1 S3 100.72(13) . 3_566
S2 Cu1 S3 108.75(5) . 3_566
S1 Cu1 S3 102.43(5) . 3_566
N1 Cu1 Mo1 141.34(13) . .
S2 Cu1 Mo1 53.03(3) . .
S1 Cu1 Mo1 51.74(3) . .
S3 Cu1 Mo1 117.93(4) 3_566 .
N1 Cu1 Cu2 120.81(12) . 3_566
S2 Cu1 Cu2 121.36(4) . 3_566
S1 Cu1 Cu2 54.11(4) . 3_566
S3 Cu1 Cu2 48.53(4) 3_566 3_566
Mo1 Cu1 Cu2 87.84(3) . 3_566
C1 Cu2 S2 117.46(13) 2_546 .
C1 Cu2 S3 120.32(13) 2_546 .
S2 Cu2 S3 104.89(4) . .
C1 Cu2 S1 100.81(14) 2_546 3_566
S2 Cu2 S1 108.71(5) . 3_566
S3 Cu2 S1 103.20(5) . 3_566
C1 Cu2 Mo1 141.51(13) 2_546 .
S2 Cu2 Mo1 52.82(3) . .
S3 Cu2 Mo1 52.08(3) . .
S1 Cu2 Mo1 117.67(4) 3_566 .
C1 Cu2 Cu1 119.22(13) 2_546 3_566
S2 Cu2 Cu1 121.77(4) . 3_566
S3 Cu2 Cu1 54.90(4) . 3_566
S1 Cu2 Cu1 48.51(4) 3_566 3_566
Mo1 Cu2 Cu1 88.13(3) . 3_566
Mo1 S1 Cu1 73.45(4) . .
Mo1 S1 Cu2 114.59(5) . 3_566
Cu1 S1 Cu2 77.38(4) . 3_566
Mo1 S2 Cu2 73.42(4) . .
Mo1 S2 Cu1 72.95(4) . .
Cu2 S2 Cu1 116.84(5) . .
Mo1 S3 Cu2 73.31(4) . .
Mo1 S3 Cu1 113.35(5) . 3_566
Cu2 S3 Cu1 76.57(4) . 3_566
C1 N1 Cu1 176.3(4) . .
C2 N2 C4 111.2(4) . .
C2 N2 C6 111.4(3) . .
C4 N2 C6 107.0(3) . .
C2 N2 C8 106.2(3) . .
C4 N2 C8 110.6(3) . .
C6 N2 C8 110.5(4) . .
C10 N3 H16 117(5) . .
C10 N3 H17 116(5) . .
H16 N3 H17 110(7) . .
N1 C1 Cu2 177.6(4) . 2_556
N2 C2 C3 114.7(4) . .
N2 C2 H2A 108.6 . .
C3 C2 H2A 108.6 . .
N2 C2 H2B 108.6 . .
C3 C2 H2B 108.6 . .
H2A C2 H2B 107.6 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N2 C4 C5 115.9(4) . .
N2 C4 H4A 108.3 . .
C5 C4 H4A 108.3 . .
N2 C4 H4B 108.3 . .
C5 C4 H4B 108.3 . .
H4A C4 H4B 107.4 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C6 C7 115.2(4) . .
N2 C6 H6A 108.5 . .
C7 C6 H6A 108.5 . .
N2 C6 H6B 108.5 . .
C7 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C9 C8 N2 115.1(4) . .
C9 C8 H8A 108.5 . .
N2 C8 H8A 108.5 . .
C9 C8 H8B 108.5 . .
N2 C8 H8B 108.5 . .
H8A C8 H8B 107.5 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N3 C10 C11 121.1(6) . .
N3 C10 C15 120.7(5) . .
C11 C10 C15 118.2(5) . .
C12 C11 C10 120.1(6) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 122.2(6) . .
C11 C12 H12 118.9 . .
C13 C12 H12 118.9 . .
C12 C13 C14 117.5(6) . .
C12 C13 H13 121.3 . .
C14 C13 H13 121.3 . .
C15 C14 C13 122.0(6) . .
C15 C14 H14 119.0 . .
C13 C14 H14 119.0 . .
C14 C15 C10 120.0(5) . .
C14 C15 H15 120.0 . .
C10 C15 H15 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.718(3) .
Mo1 S1 2.2133(12) .
Mo1 S3 2.2373(12) .
Mo1 S2 2.2580(12) .
Mo1 Cu1 2.7020(8) .
Mo1 Cu2 2.7165(8) .
Cu1 N1 1.945(4) .
Cu1 S2 2.2867(13) .
Cu1 S1 2.3036(13) .
Cu1 S3 2.5241(18) 3_566
Cu1 Cu2 3.0008(11) 3_566
Cu2 C1 1.936(4) 2_546
Cu2 S2 2.2860(13) .
Cu2 S3 2.3119(13) .
Cu2 S1 2.4911(17) 3_566
Cu2 Cu1 3.0008(11) 3_566
S1 Cu2 2.4911(17) 3_566
S3 Cu1 2.5241(17) 3_566
N1 C1 1.147(5) .
N2 C2 1.507(6) .
N2 C4 1.511(6) .
N2 C6 1.512(5) .
N2 C8 1.523(6) .
N3 C10 1.355(8) .
N3 H16 0.89(7) .
N3 H17 0.88(5) .
C1 Cu2 1.936(4) 2_556
C2 C3 1.531(7) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.520(7) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.516(6) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.510(7) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.397(7) .
C10 C15 1.397(8) .
C11 C12 1.366(8) .
C11 H11 0.9500 .
C12 C13 1.377(9) .
C12 H12 0.9500 .
C13 C14 1.377(8) .
C13 H13 0.9500 .
C14 C15 1.373(8) .
C14 H14 0.9500 .
C15 H15 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H17 O1 0.88(5) 2.19(3) 3.044(7) 162(7) .
N3 H16 O1 0.89(7) 2.16(7) 3.040(7) 171(7) 3_667
