#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:41:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179419 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/16/4331620.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_4331620
loop_
_publ_author_name
'Bo Liu'
'Jin Yang'
'Guo-Cheng Yang'
'Jian-Fang Ma'
_publ_contact_author_address
;
Key Lab of Polyoxometalate Science
Department of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       jianfangma@yahoo.com.cn
_publ_contact_author_fax         +86-431-85098620
_publ_contact_author_name        'Jian-Fang Ma'
_publ_contact_author_phone       +86-431-85098620
_publ_section_title
;
 Four New Three-Dimensional Polyoxometalate-Based Metal-Organic Frameworks
 Constructed From [Mo6O18(O3AsPh)2]4- Polyoxoanions and Copper(I)-Organic
 Fragments: Syntheses, Structures, Electrochemistry, and Photocatalysis
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              84
_journal_page_last               94
_journal_paper_doi               10.1021/ic301257k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H29 As Cu2 Mo3 N12 O12'
_chemical_formula_sum            'C22 H29 As Cu2 Mo3 N12 O12'
_chemical_formula_weight         1143.39
_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                109.716(3)
_cell_angle_beta                 96.413(2)
_cell_angle_gamma                107.931(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3976(3)
_cell_length_b                   13.3822(4)
_cell_length_c                   13.3964(5)
_cell_measurement_reflns_used    7279
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0856
_cell_measurement_theta_min      2.8582
_cell_volume                     1776.28(11)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       'ω scan'
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12306
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    3.206
_exptl_absorpt_correction_T_max  0.5524
_exptl_absorpt_correction_T_min  0.3999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6943
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0380
_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)+(0.0655P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                5199
_reflns_number_total             6943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301257k_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        1776.28(10)
_cod_database_code               4331620
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 0.48103(7) -0.01468(6) -0.13558(7) 0.0566(2) Uani 1 1 d . . .
Cu2 Cu 0.64480(9) 0.50498(7) 0.50041(8) 0.0672(3) Uani 1 1 d . . .
As1 As 0.61847(5) 0.46902(4) -0.05128(4) 0.02489(13) Uani 1 1 d . . .
Mo1 Mo 0.41393(4) 0.26147(3) 0.03926(4) 0.03287(13) Uani 1 1 d . . .
Mo2 Mo 0.61947(5) 0.49783(3) 0.23096(4) 0.03494(13) Uani 1 1 d . . .
Mo3 Mo 0.71236(4) 0.73471(3) 0.19081(4) 0.03431(13) Uani 1 1 d . . .
C1 C 0.7247(6) 0.1709(5) -0.0171(6) 0.0602(14) Uani 1 1 d U . .
H1 H 0.6860 0.2201 0.0180 0.072 Uiso 1 1 calc R . .
C2 C 0.7484(6) 0.0257(6) -0.1212(7) 0.0640(14) Uani 1 1 d U A .
H2 H 0.7338 -0.0464 -0.1730 0.077 Uiso 1 1 calc R . .
C3 C 0.9857(7) 0.0990(6) -0.0738(7) 0.0683(13) Uani 0.368(15) 1 d PDU A 1
H3A H 1.0455 0.1727 -0.0650 0.082 Uiso 0.368(15) 1 calc PR A 1
H3B H 0.9815 0.0423 -0.1437 0.082 Uiso 0.368(15) 1 calc PR A 1
C4 C 1.026(2) 0.0651(4) 0.0224(12) 0.069(2) Uani 0.368(15) 1 d PDU . 1
H4A H 1.1180 0.0949 0.0473 0.083 Uiso 0.368(15) 1 calc PR A 1
H4B H 0.9913 0.0958 0.0833 0.083 Uiso 0.368(15) 1 calc PR A 1
C3' C 0.9857(7) 0.0990(6) -0.0738(7) 0.0683(13) Uani 0.632(15) 1 d PU A 2
H3'1 H 0.9831 0.0615 -0.1504 0.082 Uiso 0.632(15) 1 calc PR A 2
H3'2 H 1.0457 0.1769 -0.0488 0.082 Uiso 0.632(15) 1 calc PR A 2
C4' C 1.0361(12) 0.0435(11) -0.0157(13) 0.070(2) Uani 0.632(15) 1 d PU . 2
H4'1 H 1.0887 0.0117 -0.0586 0.085 Uiso 0.632(15) 1 calc PR A 2
H4'2 H 1.0936 0.1040 0.0512 0.085 Uiso 0.632(15) 1 calc PR A 2
C5 C 0.2220(7) -0.0981(5) -0.2546(7) 0.0711(16) Uani 1 1 d U . .
H5 H 0.2301 -0.0240 -0.2451 0.085 Uiso 1 1 calc R . .
C6 C 0.2629(6) -0.2334(5) -0.2411(6) 0.0556(13) Uani 1 1 d U . .
H6 H 0.3037 -0.2776 -0.2231 0.067 Uiso 1 1 calc R . .
C7 C 0.0547(6) -0.3900(5) -0.3525(6) 0.0623(15) Uani 1 1 d U . .
H7A H -0.0281 -0.3911 -0.3409 0.075 Uiso 1 1 calc R . .
H7B H 0.0789 -0.4375 -0.3198 0.075 Uiso 1 1 calc R . .
C8 C 0.0462(6) -0.4382(5) -0.4718(6) 0.0596(15) Uani 1 1 d U . .
H8A H 0.1298 -0.4341 -0.4832 0.072 Uiso 1 1 calc R . .
H8B H 0.0189 -0.3922 -0.5048 0.072 Uiso 1 1 calc R . .
C9 C 0.5078(8) 0.2608(7) 0.3856(8) 0.0834(18) Uani 1 1 d U . .
H9 H 0.5053 0.2652 0.3176 0.100 Uiso 1 1 calc R . .
C10 C 0.5506(9) 0.3090(7) 0.5561(8) 0.0914(17) Uani 1 1 d U . .
H10 H 0.5807 0.3501 0.6312 0.110 Uiso 1 1 calc R . .
C11 C 0.4384(10) 0.1199(8) 0.5584(9) 0.1014(18) Uani 1 1 d U . .
H11A H 0.3502 0.0725 0.5217 0.122 Uiso 1 1 calc R . .
H11B H 0.4416 0.1632 0.6338 0.122 Uiso 1 1 calc R . .
C12 C 0.5134(10) 0.0433(8) 0.5559(8) 0.110(2) Uani 1 1 d U . .
H12A H 0.6036 0.0893 0.5808 0.131 Uiso 1 1 calc R . .
H12B H 0.4911 0.0053 0.6051 0.131 Uiso 1 1 calc R . .
C13 C 0.8118(9) 0.7295(7) 0.5161(8) 0.0886(18) Uani 1 1 d U A .
H13 H 0.8179 0.7081 0.4437 0.106 Uiso 1 1 calc R . .
C14 C 0.7740(9) 0.7282(8) 0.6659(8) 0.093(2) Uani 1 1 d U . .
H14 H 0.7457 0.7020 0.7182 0.112 Uiso 1 1 calc R . .
C15 C 0.9407(9) 0.9374(8) 0.5940(7) 0.1008(18) Uani 0.368(15) 1 d PDU A 1
H15A H 1.0274 0.9418 0.6120 0.121 Uiso 0.368(15) 1 calc PR A 1
H15B H 0.9312 0.9960 0.6555 0.121 Uiso 0.368(15) 1 calc PR A 1
C16 C 0.9297(6) 0.974(3) 0.4982(18) 0.103(3) Uani 0.368(15) 1 d PDU . 1
H16A H 0.8889 1.0290 0.5097 0.123 Uiso 0.368(15) 1 calc PR A 1
H16B H 0.8842 0.9086 0.4299 0.123 Uiso 0.368(15) 1 calc PR A 1
C15' C 0.9407(9) 0.9374(8) 0.5940(7) 0.1008(18) Uani 0.632(15) 1 d PDU A 2
H15C H 1.0149 0.9688 0.6541 0.121 Uiso 0.632(15) 1 calc PR A 2
H15D H 0.8951 0.9891 0.6103 0.121 Uiso 0.632(15) 1 calc PR A 2
C16' C 0.9851(17) 0.9367(6) 0.4932(10) 0.103(2) Uani 0.632(15) 1 d PDU . 2
H16D H 0.9193 0.8837 0.4278 0.123 Uiso 0.632(15) 1 calc PR A 2
H16C H 1.0605 0.9175 0.4913 0.123 Uiso 0.632(15) 1 calc PR A 2
C17 C 0.7539(6) 0.4377(5) -0.1104(5) 0.0453(11) Uani 1 1 d U . .
C18 C 0.7399(6) 0.3272(5) -0.1709(6) 0.0599(12) Uani 1 1 d U . .
H18 H 0.6644 0.2667 -0.1846 0.072 Uiso 1 1 calc R . .
C19 C 0.8425(7) 0.3087(6) -0.2110(6) 0.0678(14) Uani 1 1 d U . .
H19 H 0.8364 0.2346 -0.2510 0.081 Uiso 1 1 calc R . .
C20 C 0.9513(7) 0.3983(6) -0.1921(6) 0.0650(13) Uani 1 1 d U . .
H20 H 1.0183 0.3848 -0.2206 0.078 Uiso 1 1 calc R . .
C21 C 0.9637(7) 0.5058(6) -0.1332(6) 0.0693(14) Uani 1 1 d U . .
H21 H 1.0397 0.5659 -0.1188 0.083 Uiso 1 1 calc R . .
C22 C 0.8643(6) 0.5266(6) -0.0944(6) 0.0614(13) Uani 1 1 d U . .
H22 H 0.8712 0.6015 -0.0568 0.074 Uiso 1 1 calc R . .
N1 N 0.6595(4) 0.0642(4) -0.0920(4) 0.0474(12) Uani 1 1 d . . .
N2 N 0.8484(5) 0.1988(5) 0.0017(5) 0.0687(17) Uani 1 1 d . A .
N3 N 0.8604(5) 0.1035(4) -0.0670(5) 0.0573(14) Uani 1 1 d . . .
N4 N 0.3146(5) -0.1224(4) -0.2118(4) 0.0507(13) Uani 1 1 d U . .
N5 N 0.1175(6) -0.1874(5) -0.3119(6) 0.088(2) Uani 1 1 d U . .
N6 N 0.1472(5) -0.2728(4) -0.2986(5) 0.0567(14) Uani 1 1 d U . .
N7 N 0.5658(6) 0.3517(4) 0.4801(4) 0.0583(14) Uani 1 1 d . . .
N8 N 0.4540(7) 0.1635(6) 0.3981(6) 0.0829(19) Uani 1 1 d U . .
N9 N 0.4856(7) 0.1986(5) 0.5068(6) 0.0779(18) Uani 1 1 d U . .
N10 N 0.7498(6) 0.6598(5) 0.5592(5) 0.0667(16) Uani 1 1 d . . .
N11 N 0.8633(7) 0.8334(5) 0.5914(7) 0.087(2) Uani 1 1 d . . .
N12 N 0.8409(8) 0.8342(7) 0.6875(7) 0.105(3) Uani 1 1 d . A .
O1 O 0.4345(4) 0.1381(3) -0.0333(3) 0.0482(10) Uani 1 1 d . . .
O2 O 0.3425(4) 0.2316(3) 0.1360(3) 0.0511(10) Uani 1 1 d . . .
O3 O 0.4999(3) 0.3431(2) -0.0796(3) 0.0289(7) Uani 1 1 d . . .
O4 O 0.5841(3) 0.3478(3) 0.1258(3) 0.0369(8) Uani 1 1 d . . .
O5 O 0.4293(3) 0.4515(2) 0.1109(3) 0.0293(7) Uani 1 1 d . . .
O6 O 0.5382(4) 0.4682(3) 0.3244(3) 0.0536(11) Uani 1 1 d . . .
O7 O 0.7721(4) 0.5250(3) 0.2892(3) 0.0576(12) Uani 1 1 d . . .
O8 O 0.6757(3) 0.5462(3) 0.0865(3) 0.0303(7) Uani 1 1 d . . .
O9 O 0.6247(3) 0.6496(3) 0.2670(3) 0.0348(8) Uani 1 1 d . . .
O10 O 0.6917(4) 0.8586(3) 0.2584(3) 0.0516(11) Uani 1 1 d . . .
O11 O 0.8657(4) 0.7611(3) 0.2454(4) 0.0583(12) Uani 1 1 d . . .
O12 O 0.7299(3) 0.7488(3) 0.0564(3) 0.0337(8) Uani 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'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
N1 Cu1 N4 163.6(2) . .
N1 Cu1 O1 95.23(17) . .
N4 Cu1 O1 100.31(18) . .
N10 Cu2 N7 162.9(3) . .
N10 Cu2 O6 105.5(2) . .
N7 Cu2 O6 91.4(2) . .
O3 As1 O5 111.49(16) . 2_665
O3 As1 O8 111.63(16) . .
O5 As1 O8 109.77(15) 2_665 .
O3 As1 C17 108.3(2) . .
O5 As1 C17 107.4(2) 2_665 .
O8 As1 C17 108.2(2) . .
O2 Mo1 O1 104.04(19) . .
O2 Mo1 O12 98.89(19) . 2_665
O1 Mo1 O12 101.31(17) . 2_665
O2 Mo1 O4 99.46(19) . .
O1 Mo1 O4 98.30(17) . .
O12 Mo1 O4 148.91(14) 2_665 .
O2 Mo1 O5 92.55(16) . .
O1 Mo1 O5 162.83(16) . .
O12 Mo1 O5 80.03(12) 2_665 .
O4 Mo1 O5 74.29(12) . .
O2 Mo1 O3 165.88(15) . .
O1 Mo1 O3 89.84(16) . .
O12 Mo1 O3 75.49(13) 2_665 .
O4 Mo1 O3 80.71(13) . .
O5 Mo1 O3 73.82(11) . .
O7 Mo2 O6 103.4(2) . .
O7 Mo2 O9 100.14(17) . .
O6 Mo2 O9 97.41(16) . .
O7 Mo2 O4 97.07(17) . .
O6 Mo2 O4 101.37(17) . .
O9 Mo2 O4 150.78(15) . .
O7 Mo2 O5 165.36(18) . .
O6 Mo2 O5 90.25(18) . .
O9 Mo2 O5 83.08(13) . .
O4 Mo2 O5 74.70(13) . .
O7 Mo2 O8 92.74(19) . .
O6 Mo2 O8 163.03(18) . .
O9 Mo2 O8 74.24(12) . .
O4 Mo2 O8 81.54(13) . .
O5 Mo2 O8 74.27(12) . .
O11 Mo3 O10 104.1(2) . .
O11 Mo3 O12 99.31(19) . .
O10 Mo3 O12 100.17(17) . .
O11 Mo3 O9 101.36(19) . .
O10 Mo3 O9 97.05(16) . .
O12 Mo3 O9 148.88(14) . .
O11 Mo3 O8 92.10(17) . .
O10 Mo3 O8 163.07(17) . .
O12 Mo3 O8 81.59(13) . .
O9 Mo3 O8 74.67(12) . .
O11 Mo3 O3 165.62(16) . 2_665
O10 Mo3 O3 89.86(17) . 2_665
O12 Mo3 O3 74.52(13) . 2_665
O9 Mo3 O3 79.82(14) . 2_665
O8 Mo3 O3 74.28(11) . 2_665
N2 C1 N1 113.4(6) . .
N2 C1 H1 123.3 . .
N1 C1 H1 123.3 . .
N3 C2 N1 110.1(6) . .
N3 C2 H2 125.0 . .
N1 C2 H2 125.0 . .
N3 C3 C4 104.8(11) . .
N3 C3 H3A 110.8 . .
C4 C3 H3A 110.8 . .
N3 C3 H3B 110.8 . .
C4 C3 H3B 110.8 . .
H3A C3 H3B 108.9 . .
C4 C4 C3 106.7(12) 2_755 .
C4 C4 H4A 110.4 2_755 .
C3 C4 H4A 110.4 . .
C4 C4 H4B 110.4 2_755 .
C3 C4 H4B 110.4 . .
H4A C4 H4B 108.6 . .
C4' C4' H4'1 105.8 2_755 .
C4' C4' H4'2 105.8 2_755 .
H4'1 C4' H4'2 106.2 . .
N5 C5 N4 114.6(6) . .
N5 C5 H5 122.7 . .
N4 C5 H5 122.7 . .
N6 C6 N4 110.6(5) . .
N6 C6 H6 124.7 . .
N4 C6 H6 124.7 . .
N6 C7 C8 112.0(6) . .
N6 C7 H7A 109.2 . .
C8 C7 H7A 109.2 . .
N6 C7 H7B 109.2 . .
C8 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
C7 C8 C8 112.5(7) . 2_544
C7 C8 H8A 109.1 . .
C8 C8 H8A 109.1 2_544 .
C7 C8 H8B 109.1 . .
C8 C8 H8B 109.1 2_544 .
H8A C8 H8B 107.8 . .
N8 C9 N7 113.8(8) . .
N8 C9 H9 123.1 . .
N7 C9 H9 123.1 . .
N9 C10 N7 108.1(8) . .
N9 C10 H10 126.0 . .
N7 C10 H10 126.0 . .
N9 C11 C12 113.1(8) . .
N9 C11 H11A 109.0 . .
C12 C11 H11A 109.0 . .
N9 C11 H11B 109.0 . .
C12 C11 H11B 109.0 . .
H11A C11 H11B 107.8 . .
C12 C12 C11 110.7(12) 2_656 .
C12 C12 H12A 109.5 2_656 .
C11 C12 H12A 109.5 . .
C12 C12 H12B 109.5 2_656 .
C11 C12 H12B 109.5 . .
H12A C12 H12B 108.1 . .
N11 C13 N10 109.2(9) . .
N11 C13 H13 125.4 . .
N10 C13 H13 125.4 . .
N12 C14 N10 112.9(9) . .
N12 C14 H14 123.6 . .
N10 C14 H14 123.6 . .
N11 C15 C16 123.5(11) . .
N11 C15 H15A 106.5 . .
C16 C15 H15A 106.5 . .
N11 C15 H15B 106.5 . .
C16 C15 H15B 106.5 . .
H15A C15 H15B 106.5 . .
C15 C16 C16 99.8(12) . 2_776
C15 C16 H16A 111.8 . .
C16 C16 H16A 111.8 2_776 .
C15 C16 H16B 111.8 . .
C16 C16 H16B 111.8 2_776 .
H16A C16 H16B 109.5 . .
C16' C16' H16D 111.5 2_776 .
C16' C16' H16C 111.5 2_776 .
H16D C16' H16C 109.3 . .
C18 C17 C22 120.4(5) . .
C18 C17 As1 120.1(4) . .
C22 C17 As1 119.5(4) . .
C17 C18 C19 117.8(6) . .
C17 C18 H18 121.1 . .
C19 C18 H18 121.1 . .
C20 C19 C18 120.4(6) . .
C20 C19 H19 119.8 . .
C18 C19 H19 119.8 . .
C21 C20 C19 121.2(6) . .
C21 C20 H20 119.4 . .
C19 C20 H20 119.4 . .
C20 C21 C22 119.7(7) . .
C20 C21 H21 120.1 . .
C22 C21 H21 120.1 . .
C21 C22 C17 120.4(6) . .
C21 C22 H22 119.8 . .
C17 C22 H22 119.8 . .
C2 N1 C1 103.8(5) . .
C2 N1 Cu1 128.5(4) . .
C1 N1 Cu1 127.5(4) . .
C1 N2 N3 102.6(5) . .
C2 N3 N2 110.1(5) . .
C2 N3 C3 129.1(6) . .
N2 N3 C3 120.7(5) . .
C6 N4 C5 102.9(5) . .
C6 N4 Cu1 132.2(4) . .
C5 N4 Cu1 124.7(4) . .
C5 N5 N6 101.6(6) . .
C6 N6 N5 110.1(5) . .
C6 N6 C7 130.6(5) . .
N5 N6 C7 119.2(5) . .
C10 N7 C9 104.2(7) . .
C10 N7 Cu2 127.9(6) . .
C9 N7 Cu2 127.9(5) . .
C9 N8 N9 101.4(7) . .
C10 N9 N8 112.6(7) . .
C10 N9 C11 126.8(8) . .
N8 N9 C11 120.4(7) . .
C13 N10 C14 103.6(7) . .
C13 N10 Cu2 133.3(6) . .
C14 N10 Cu2 123.0(6) . .
C13 N11 N12 110.4(8) . .
C13 N11 C15 134.3(10) . .
N12 N11 C15 115.2(7) . .
C14 N12 N11 103.9(7) . .
Mo1 O1 Cu1 173.5(2) . .
As1 O3 Mo1 130.01(17) . .
As1 O3 Mo3 129.73(17) . 2_665
Mo1 O3 Mo3 87.09(10) . 2_665
Mo2 O4 Mo1 117.77(18) . .
As1 O5 Mo2 129.80(16) 2_665 .
As1 O5 Mo1 131.31(18) 2_665 .
Mo2 O5 Mo1 89.21(11) . .
Mo2 O6 Cu2 121.5(2) . .
As1 O8 Mo3 130.60(18) . .
As1 O8 Mo2 129.48(16) . .
Mo3 O8 Mo2 89.43(11) . .
Mo2 O9 Mo3 117.95(17) . .
Mo3 O12 Mo1 119.05(17) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.895(5) .
Cu1 N4 1.900(5) .
Cu1 O1 2.298(4) .
Cu2 N10 1.873(6) .
Cu2 N7 1.878(5) .
Cu2 O6 2.342(4) .
As1 O3 1.691(3) .
As1 O5 1.703(3) 2_665
As1 O8 1.711(3) .
As1 C17 1.906(5) .
Mo1 O2 1.700(4) .
Mo1 O1 1.712(3) .
Mo1 O12 1.903(4) 2_665
Mo1 O4 1.912(4) .
Mo1 O5 2.337(3) .
Mo1 O3 2.357(3) .
Mo2 O7 1.698(4) .
Mo2 O6 1.718(4) .
Mo2 O9 1.902(3) .
Mo2 O4 1.909(3) .
Mo2 O5 2.322(3) .
Mo2 O8 2.333(3) .
Mo3 O11 1.696(4) .
Mo3 O10 1.703(3) .
Mo3 O12 1.898(4) .
Mo3 O9 1.910(3) .
Mo3 O8 2.310(3) .
Mo3 O3 2.399(3) 2_665
C1 N2 1.313(8) .
C1 N1 1.346(8) .
C1 H1 0.9300 .
C2 N3 1.306(8) .
C2 N1 1.310(8) .
C2 H2 0.9300 .
C3 N3 1.460(8) .
C3 C4 1.571(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C4 1.525(10) 2_755
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4' C4' 1.42(2) 2_755
C4' H4'1 0.9700 .
C4' H4'2 0.9700 .
C5 N5 1.318(8) .
C5 N4 1.322(8) .
C5 H5 0.9300 .
C6 N6 1.296(8) .
C6 N4 1.313(7) .
C6 H6 0.9300 .
C7 N6 1.463(7) .
C7 C8 1.487(10) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C8 1.524(11) 2_544
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 N8 1.333(10) .
C9 N7 1.341(9) .
C9 H9 0.9300 .
C10 N9 1.314(10) .
C10 N7 1.328(10) .
C10 H10 0.9300 .
C11 N9 1.450(11) .
C11 C12 1.518(13) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C12 1.480(18) 2_656
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 N11 1.309(10) .
C13 N10 1.324(11) .
C13 H13 0.9300 .
C14 N12 1.299(11) .
C14 N10 1.353(10) .
C14 H14 0.9300 .
C15 N11 1.386(10) .
C15 C16 1.522(10) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C16 1.527(10) 2_776
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16' C16' 1.564(10) 2_776
C16' H16D 0.9700 .
C16' H16C 0.9700 .
C17 C18 1.373(8) .
C17 C22 1.375(8) .
C18 C19 1.396(9) .
C18 H18 0.9300 .
C19 C20 1.360(9) .
C19 H19 0.9300 .
C20 C21 1.340(9) .
C20 H20 0.9300 .
C21 C22 1.364(9) .
C21 H21 0.9300 .
C22 H22 0.9300 .
N2 N3 1.354(7) .
N5 N6 1.348(7) .
N8 N9 1.337(9) .
N11 N12 1.337(11) .
O3 Mo3 2.399(3) 2_665
O5 As1 1.703(3) 2_665
O12 Mo1 1.903(4) 2_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N3 C3 C4 C4 88(2) . 2_755
N6 C7 C8 C8 177.8(7) . 2_544
N9 C11 C12 C12 -72.1(14) . 2_656
N11 C15 C16 C16 -137(2) . 2_776
O3 As1 C17 C18 4.2(6) . .
O5 As1 C17 C18 -116.3(6) 2_665 .
O8 As1 C17 C18 125.3(6) . .
O3 As1 C17 C22 -177.4(5) . .
O5 As1 C17 C22 62.1(6) 2_665 .
O8 As1 C17 C22 -56.3(6) . .
C22 C17 C18 C19 2.5(11) . .
As1 C17 C18 C19 -179.1(6) . .
C17 C18 C19 C20 -1.4(12) . .
C18 C19 C20 C21 1.2(13) . .
C19 C20 C21 C22 -2.2(13) . .
C20 C21 C22 C17 3.4(13) . .
C18 C17 C22 C21 -3.6(12) . .
As1 C17 C22 C21 178.0(6) . .
N3 C2 N1 C1 0.5(8) . .
N3 C2 N1 Cu1 -175.1(5) . .
N2 C1 N1 C2 -0.7(8) . .
N2 C1 N1 Cu1 174.9(5) . .
N4 Cu1 N1 C2 -18.3(12) . .
O1 Cu1 N1 C2 179.9(6) . .
N4 Cu1 N1 C1 167.2(7) . .
O1 Cu1 N1 C1 5.4(6) . .
N1 C1 N2 N3 0.7(8) . .
N1 C2 N3 N2 -0.1(9) . .
N1 C2 N3 C3 -179.0(7) . .
C1 N2 N3 C2 -0.3(8) . .
C1 N2 N3 C3 178.7(7) . .
C4 C3 N3 C2 -97.1(8) . .
C4 C3 N3 N2 84.1(7) . .
N6 C6 N4 C5 0.6(8) . .
N6 C6 N4 Cu1 -175.9(5) . .
N5 C5 N4 C6 -2.3(10) . .
N5 C5 N4 Cu1 174.5(6) . .
N1 Cu1 N4 C6 55.8(12) . .
O1 Cu1 N4 C6 -142.6(6) . .
N1 Cu1 N4 C5 -120.0(8) . .
O1 Cu1 N4 C5 41.6(6) . .
N4 C5 N5 N6 2.9(10) . .
N4 C6 N6 N5 1.2(9) . .
N4 C6 N6 C7 177.1(7) . .
C5 N5 N6 C6 -2.4(9) . .
C5 N5 N6 C7 -178.8(7) . .
C8 C7 N6 C6 -100.9(9) . .
C8 C7 N6 N5 74.6(9) . .
N9 C10 N7 C9 -0.5(9) . .
N9 C10 N7 Cu2 177.3(5) . .
N8 C9 N7 C10 1.6(10) . .
N8 C9 N7 Cu2 -176.2(5) . .
N10 Cu2 N7 C10 27.1(13) . .
O6 Cu2 N7 C10 -159.2(7) . .
N10 Cu2 N7 C9 -155.6(8) . .
O6 Cu2 N7 C9 18.1(7) . .
N7 C9 N8 N9 -1.9(9) . .
N7 C10 N9 N8 -0.7(10) . .
N7 C10 N9 C11 -174.5(8) . .
C9 N8 N9 C10 1.5(9) . .
C9 N8 N9 C11 175.9(8) . .
C12 C11 N9 C10 -106.0(11) . .
C12 C11 N9 N8 80.6(11) . .
N11 C13 N10 C14 -3.2(10) . .
N11 C13 N10 Cu2 174.4(5) . .
N12 C14 N10 C13 3.0(10) . .
N12 C14 N10 Cu2 -174.9(6) . .
N7 Cu2 N10 C13 140.5(9) . .
O6 Cu2 N10 C13 -33.0(8) . .
N7 Cu2 N10 C14 -42.3(12) . .
O6 Cu2 N10 C14 144.2(6) . .
N10 C13 N11 N12 2.5(11) . .
N10 C13 N11 C15 177.2(9) . .
C16 C15 N11 C13 36.0(19) . .
C16 C15 N11 N12 -149.4(14) . .
N10 C14 N12 N11 -1.6(11) . .
C13 N11 N12 C14 -0.6(10) . .
C15 N11 N12 C14 -176.4(8) . .
O2 Mo1 O1 Cu1 -154(2) . .
O12 Mo1 O1 Cu1 103(2) 2_665 .
O4 Mo1 O1 Cu1 -52(2) . .
O5 Mo1 O1 Cu1 11(3) . .
O3 Mo1 O1 Cu1 28(2) . .
N1 Cu1 O1 Mo1 37(2) . .
N4 Cu1 O1 Mo1 -138(2) . .
O5 As1 O3 Mo1 -125.8(2) 2_665 .
O8 As1 O3 Mo1 -2.7(3) . .
C17 As1 O3 Mo1 116.3(3) . .
O5 As1 O3 Mo3 1.8(3) 2_665 2_665
O8 As1 O3 Mo3 125.0(2) . 2_665
C17 As1 O3 Mo3 -116.0(3) . 2_665
O2 Mo1 O3 As1 62.0(8) . .
O1 Mo1 O3 As1 -128.3(2) . .
O12 Mo1 O3 As1 130.0(2) 2_665 .
O4 Mo1 O3 As1 -29.8(2) . .
O5 Mo1 O3 As1 46.4(2) . .
O2 Mo1 O3 Mo3 -80.4(7) . 2_665
O1 Mo1 O3 Mo3 89.28(15) . 2_665
O12 Mo1 O3 Mo3 -12.45(11) 2_665 2_665
O4 Mo1 O3 Mo3 -172.29(12) . 2_665
O5 Mo1 O3 Mo3 -96.07(11) . 2_665
O7 Mo2 O4 Mo1 174.2(2) . .
O6 Mo2 O4 Mo1 69.0(2) . .
O9 Mo2 O4 Mo1 -60.0(4) . .
O5 Mo2 O4 Mo1 -18.14(17) . .
O8 Mo2 O4 Mo1 -94.0(2) . .
O2 Mo1 O4 Mo2 -71.9(2) . .
O1 Mo1 O4 Mo2 -177.8(2) . .
O12 Mo1 O4 Mo2 53.5(4) 2_665 .
O5 Mo1 O4 Mo2 18.06(17) . .
O3 Mo1 O4 Mo2 93.74(19) . .
O7 Mo2 O5 As1 -77.8(6) . 2_665
O6 Mo2 O5 As1 123.3(2) . 2_665
O9 Mo2 O5 As1 25.9(2) . 2_665
O4 Mo2 O5 As1 -134.9(3) . 2_665
O8 Mo2 O5 As1 -49.6(2) . 2_665
O7 Mo2 O5 Mo1 70.2(6) . .
O6 Mo2 O5 Mo1 -88.69(15) . .
O9 Mo2 O5 Mo1 173.88(13) . .
O4 Mo2 O5 Mo1 13.03(13) . .
O8 Mo2 O5 Mo1 98.36(12) . .
O2 Mo1 O5 As1 -126.8(3) . 2_665
O1 Mo1 O5 As1 67.9(6) . 2_665
O12 Mo1 O5 As1 -28.2(2) 2_665 2_665
O4 Mo1 O5 As1 134.1(3) . 2_665
O3 Mo1 O5 As1 49.5(2) . 2_665
O2 Mo1 O5 Mo2 86.07(17) . .
O1 Mo1 O5 Mo2 -79.3(6) . .
O12 Mo1 O5 Mo2 -175.35(14) 2_665 .
O4 Mo1 O5 Mo2 -13.04(13) . .
O3 Mo1 O5 Mo2 -97.70(12) . .
O7 Mo2 O6 Cu2 11.8(3) . .
O9 Mo2 O6 Cu2 -90.6(2) . .
O4 Mo2 O6 Cu2 111.9(2) . .
O5 Mo2 O6 Cu2 -173.6(2) . .
O8 Mo2 O6 Cu2 -149.7(4) . .
N10 Cu2 O6 Mo2 55.1(3) . .
N7 Cu2 O6 Mo2 -123.0(3) . .
O3 As1 O8 Mo3 -130.7(2) . .
O5 As1 O8 Mo3 -6.5(3) 2_665 .
C17 As1 O8 Mo3 110.3(3) . .
O3 As1 O8 Mo2 2.9(3) . .
O5 As1 O8 Mo2 127.1(2) 2_665 .
C17 As1 O8 Mo2 -116.1(3) . .
O11 Mo3 O8 As1 -125.3(3) . .
O10 Mo3 O8 As1 71.1(6) . .
O12 Mo3 O8 As1 -26.2(2) . .
O9 Mo3 O8 As1 133.5(3) . .
O3 Mo3 O8 As1 50.0(2) 2_665 .
O11 Mo3 O8 Mo2 88.74(18) . .
O10 Mo3 O8 Mo2 -74.9(6) . .
O12 Mo3 O8 Mo2 -172.15(14) . .
O9 Mo3 O8 Mo2 -12.46(13) . .
O3 Mo3 O8 Mo2 -95.96(12) 2_665 .
O7 Mo2 O8 As1 126.2(2) . .
O6 Mo2 O8 As1 -71.9(6) . .
O9 Mo2 O8 As1 -134.1(3) . .
O4 Mo2 O8 As1 29.4(2) . .
O5 Mo2 O8 As1 -47.0(2) . .
O7 Mo2 O8 Mo3 -87.22(15) . .
O6 Mo2 O8 Mo3 74.8(5) . .
O9 Mo2 O8 Mo3 12.54(13) . .
O4 Mo2 O8 Mo3 176.04(14) . .
O5 Mo2 O8 Mo3 99.65(12) . .
O7 Mo2 O9 Mo3 72.7(3) . .
O6 Mo2 O9 Mo3 177.8(2) . .
O4 Mo2 O9 Mo3 -52.4(4) . .
O5 Mo2 O9 Mo3 -92.8(2) . .
O8 Mo2 O9 Mo3 -17.30(18) . .
O11 Mo3 O9 Mo2 -71.6(2) . .
O10 Mo3 O9 Mo2 -177.6(2) . .
O12 Mo3 O9 Mo2 59.1(4) . .
O8 Mo3 O9 Mo2 17.44(18) . .
O3 Mo3 O9 Mo2 93.8(2) 2_665 .
O11 Mo3 O12 Mo1 -175.43(19) . 2_665
O10 Mo3 O12 Mo1 -69.1(2) . 2_665
O9 Mo3 O12 Mo1 53.4(4) . 2_665
O8 Mo3 O12 Mo1 93.81(18) . 2_665
O3 Mo3 O12 Mo1 17.89(15) 2_665 2_665
