#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:22:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179107 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/69/4306929.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_4306929
loop_
_publ_author_name
'Chunyan Sun'
'Yangguang Li'
'Enbo Wang'
'Dongrong Xiao'
'Haiyan An'
'Lin Xu'
_publ_section_title
;
A Series of New Organic-Inorganic Molybdenum Arsenate Complexes Based on
[(ZnO6)(As3O3)2Mo6O18]4- and [HxAs2Mo6O26](6-x)- Clusters as SBUs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1563
_journal_page_last               1574
_journal_paper_doi               10.1021/ic061227j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C20 H42 As6 Mo6 N4 O42 Zn2'
_chemical_formula_weight         2166.48
_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                114.93(3)
_cell_angle_beta                 93.63(3)
_cell_angle_gamma                105.82(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3252(19)
_cell_length_b                   12.051(2)
_cell_length_c                   14.174(3)
_cell_measurement_reflns_used    4555
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.07
_cell_volume                     1360.4(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP diffractomete'
_diffrn_measurement_method       'Oscillation 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  0.1089
_diffrn_reflns_av_sigmaI/netI    0.1523
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.935
_exptl_absorpt_correction_T_max  0.271
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0783
_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)+(0.0738P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                2596
_reflns_number_total             4555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061227jsi20060704_031318.cif
_cod_data_source_block           s64e
_cod_original_cell_volume        1360.4(5)
_cod_database_code               4306929
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
Mo1 Mo 0.10911(12) 0.25909(13) 0.24131(9) 0.0264(3) Uani 1 1 d . . .
Mo2 Mo 0.00610(12) -0.04175(13) 0.22042(9) 0.0258(3) Uani 1 1 d . . .
Mo3 Mo -0.11640(12) -0.30034(13) -0.01881(10) 0.0253(3) Uani 1 1 d . . .
As1 As 0.35038(14) 0.07374(16) 0.15002(11) 0.0282(4) Uani 1 1 d . . .
As2 As 0.34309(14) 0.10347(16) -0.06789(12) 0.0276(4) Uani 1 1 d . . .
As3 As 0.23775(14) -0.18516(15) -0.07902(12) 0.0278(4) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.0000 0.0000 0.0218(5) Uani 1 2 d S . .
O1 O 0.1550(8) 0.0662(9) 0.1396(6) 0.021(2) Uani 1 1 d U . .
O2 O 0.0521(9) -0.1736(9) -0.0761(7) 0.024(2) Uani 1 1 d U . .
O3 O 0.1520(8) 0.0992(8) -0.0616(6) 0.0164(19) Uani 1 1 d . . .
O4 O 0.3220(10) -0.0905(10) 0.0595(8) 0.032(2) Uani 1 1 d . . .
O5 O 0.4098(8) 0.1519(9) 0.0683(7) 0.025(2) Uani 1 1 d U . .
O6 O 0.3159(9) -0.0661(10) -0.1240(7) 0.026(2) Uani 1 1 d . . .
O7 O -0.0257(9) 0.1220(10) 0.2606(7) 0.026(2) Uani 1 1 d . . .
O8 O 0.0301(9) -0.1951(11) 0.1126(7) 0.030(2) Uani 1 1 d . . .
O9 O 0.2671(10) 0.3074(11) 0.3359(8) 0.043(3) Uani 1 1 d . . .
O10 O 0.0201(13) 0.3732(11) 0.2926(8) 0.042(3) Uani 1 1 d . . .
O11 O 0.1658(11) 0.0056(11) 0.3136(8) 0.041(3) Uani 1 1 d . . .
O12 O -0.1434(11) -0.1105(11) 0.2627(8) 0.038(3) Uani 1 1 d . . .
O13 O -0.2761(10) -0.3624(11) 0.0185(8) 0.036(3) Uani 1 1 d . . .
O14 O -0.2209(9) -0.3170(10) -0.1492(7) 0.030(2) Uani 1 1 d . . .
O15 O -0.0410(10) -0.4226(11) -0.0679(8) 0.039(3) Uani 1 1 d . . .
Zn2 Zn 0.5000 0.0000 0.5000 0.0358(7) Uani 1 2 d S . .
N1 N 0.7285(11) 0.1345(14) 0.5559(9) 0.036(3) Uani 1 1 d U . .
N2 N 1.4796(12) 0.5522(13) 0.7848(11) 0.039(3) Uani 1 1 d U . .
H2A H 1.5727 0.6012 0.8130 0.039 Uiso 1 1 calc R . .
C1 C 0.7586(15) 0.2505(16) 0.6426(12) 0.035(4) Uani 1 1 d U . .
H1 H 0.6780 0.2750 0.6702 0.035 Uiso 1 1 calc R . .
C2 C 0.9049(17) 0.3328(19) 0.6907(14) 0.049(4) Uani 1 1 d U . .
H2 H 0.9233 0.4075 0.7544 0.049 Uiso 1 1 calc R . .
C3 C 1.0289(15) 0.3035(16) 0.6426(11) 0.030(3) Uani 1 1 d U . .
C4 C 0.9919(15) 0.1868(16) 0.5529(12) 0.035(4) Uani 1 1 d U . .
H4 H 1.0680 0.1618 0.5188 0.035 Uiso 1 1 calc R . .
C5 C 0.8397(14) 0.1050(17) 0.5123(12) 0.035(4) Uani 1 1 d U . .
H5 H 0.8177 0.0264 0.4516 0.035 Uiso 1 1 calc R . .
C6 C 1.3831(15) 0.5408(16) 0.8475(12) 0.037(4) Uani 1 1 d U . .
H6 H 1.4146 0.5854 0.9210 0.037 Uiso 1 1 calc R . .
C7 C 1.2320(17) 0.4597(18) 0.7999(12) 0.042(4) Uani 1 1 d U . .
H7 H 1.1628 0.4527 0.8432 0.042 Uiso 1 1 calc R . .
C8 C 1.1835(15) 0.3911(17) 0.6931(12) 0.035(4) Uani 1 1 d U . .
C9 C 1.2883(18) 0.4101(19) 0.6279(14) 0.051(5) Uani 1 1 d U . .
H9 H 1.2572 0.3702 0.5544 0.051 Uiso 1 1 calc R . .
C10 C 1.435(2) 0.4878(19) 0.6755(15) 0.055(5) Uani 1 1 d U . .
H10 H 1.5060 0.4976 0.6338 0.055 Uiso 1 1 calc R . .
OW1 O 0.4087(16) 0.1527(18) 0.5297(15) 0.101(5) Uani 1 1 d U . .
OW2 O 0.4938(18) 0.0281(18) 0.6534(12) 0.101(5) Uani 1 1 d U . .
OW3 O 0.2705(13) -0.3291(13) 0.0888(10) 0.056(3) Uani 1 1 d U . .
OW4 O 0.4637(14) 0.2817(15) 0.7803(11) 0.066(4) Uani 1 1 d U . .
OW5 O 0.2912(18) -0.1854(19) -0.3457(13) 0.064(5) Uani 0.76 1 d PU A 1
OW5A O 0.284(6) -0.309(6) -0.361(4) 0.060(14) Uani 0.24 1 d PU B 2
OW6 O 0.5266(19) 0.324(2) 0.4649(14) 0.104(6) Uani 1 1 d U . .
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'
Zn Zn 0.2839 1.4301 '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
_geom_angle_publ_flag
O9 Mo1 O10 106.2(6) . . ?
O9 Mo1 O7 101.2(4) . . ?
O10 Mo1 O7 99.0(4) . . ?
O9 Mo1 O14 95.1(4) . 2 ?
O10 Mo1 O14 101.3(4) . 2 ?
O7 Mo1 O14 149.3(4) . 2 ?
O9 Mo1 O2 161.4(4) . 2 ?
O10 Mo1 O2 88.9(5) . 2 ?
O7 Mo1 O2 86.8(3) . 2 ?
O14 Mo1 O2 70.8(3) 2 2 ?
O9 Mo1 O1 90.3(4) . . ?
O10 Mo1 O1 162.4(4) . . ?
O7 Mo1 O1 71.1(3) . . ?
O14 Mo1 O1 83.0(4) 2 . ?
O2 Mo1 O1 76.3(3) 2 . ?
O11 Mo2 O12 106.5(5) . . ?
O11 Mo2 O7 100.2(5) . . ?
O12 Mo2 O7 97.7(5) . . ?
O11 Mo2 O8 98.8(5) . . ?
O12 Mo2 O8 99.9(5) . . ?
O7 Mo2 O8 149.3(4) . . ?
O11 Mo2 O3 161.6(4) . 2 ?
O12 Mo2 O3 91.0(4) . 2 ?
O7 Mo2 O3 82.6(3) . 2 ?
O8 Mo2 O3 72.1(3) . 2 ?
O11 Mo2 O1 88.6(4) . . ?
O12 Mo2 O1 162.9(4) . . ?
O7 Mo2 O1 71.3(3) . . ?
O8 Mo2 O1 85.2(4) . . ?
O3 Mo2 O1 74.9(3) 2 . ?
O15 Mo3 O13 105.0(5) . . ?
O15 Mo3 O8 96.9(5) . . ?
O13 Mo3 O8 103.6(4) . . ?
O15 Mo3 O14 100.8(4) . . ?
O13 Mo3 O14 95.9(4) . . ?
O8 Mo3 O14 149.2(4) . . ?
O15 Mo3 O2 92.8(4) . . ?
O13 Mo3 O2 160.2(4) . . ?
O8 Mo3 O2 82.5(4) . . ?
O14 Mo3 O2 71.7(3) . . ?
O15 Mo3 O3 164.8(4) . 2 ?
O13 Mo3 O3 88.0(4) . 2 ?
O8 Mo3 O3 72.0(4) . 2 ?
O14 Mo3 O3 85.3(4) . 2 ?
O2 Mo3 O3 75.8(3) . 2 ?
O4 As1 O1 98.3(4) . . ?
O4 As1 O5 100.6(4) . . ?
O1 As1 O5 99.9(4) . . ?
O5 As2 O3 98.0(4) . . ?
O5 As2 O6 100.5(4) . . ?
O3 As2 O6 99.8(4) . . ?
O4 As3 O2 99.7(4) . . ?
O4 As3 O6 99.2(4) . . ?
O2 As3 O6 98.9(4) . . ?
O1 Zn1 O1 180.0(5) 2 . ?
O1 Zn1 O3 94.1(3) 2 2 ?
O1 Zn1 O3 85.9(3) . 2 ?
O1 Zn1 O3 85.9(3) 2 . ?
O1 Zn1 O3 94.1(3) . . ?
O3 Zn1 O3 180.0(6) 2 . ?
O1 Zn1 O2 86.9(3) 2 . ?
O1 Zn1 O2 93.1(3) . . ?
O3 Zn1 O2 85.8(3) 2 . ?
O3 Zn1 O2 94.2(3) . . ?
O1 Zn1 O2 93.1(3) 2 2 ?
O1 Zn1 O2 86.9(3) . 2 ?
O3 Zn1 O2 94.2(3) 2 2 ?
O3 Zn1 O2 85.8(3) . 2 ?
O2 Zn1 O2 180.0(7) . 2 ?
As1 O1 Zn1 126.1(4) . . ?
As1 O1 Mo2 116.8(5) . . ?
Zn1 O1 Mo2 99.6(3) . . ?
As1 O1 Mo1 116.4(4) . . ?
Zn1 O1 Mo1 99.0(4) . . ?
Mo2 O1 Mo1 92.4(3) . . ?
As3 O2 Zn1 125.8(5) . . ?
As3 O2 Mo3 118.4(5) . . ?
Zn1 O2 Mo3 98.8(3) . . ?
As3 O2 Mo1 116.2(4) . 2 ?
Zn1 O2 Mo1 97.7(4) . 2 ?
Mo3 O2 Mo1 93.6(3) . 2 ?
As2 O3 Zn1 127.3(5) . . ?
As2 O3 Mo2 116.3(4) . 2 ?
Zn1 O3 Mo2 99.5(3) . 2 ?
As2 O3 Mo3 115.8(4) . 2 ?
Zn1 O3 Mo3 99.5(3) . 2 ?
Mo2 O3 Mo3 91.6(3) 2 2 ?
As3 O4 As1 131.9(6) . . ?
As2 O5 As1 130.8(5) . . ?
As2 O6 As3 131.7(5) . . ?
Mo2 O7 Mo1 122.3(4) . . ?
Mo3 O8 Mo2 121.0(4) . . ?
Mo3 O14 Mo1 121.4(4) . 2 ?
OW2 Zn2 OW2 180.000(1) . 2_656 ?
OW2 Zn2 OW1 89.1(8) . . ?
OW2 Zn2 OW1 90.9(8) 2_656 . ?
OW2 Zn2 OW1 90.9(8) . 2_656 ?
OW2 Zn2 OW1 89.1(8) 2_656 2_656 ?
OW1 Zn2 OW1 180.000(3) . 2_656 ?
OW2 Zn2 N1 91.2(5) . 2_656 ?
OW2 Zn2 N1 88.8(5) 2_656 2_656 ?
OW1 Zn2 N1 88.7(6) . 2_656 ?
OW1 Zn2 N1 91.3(6) 2_656 2_656 ?
OW2 Zn2 N1 88.8(5) . . ?
OW2 Zn2 N1 91.2(5) 2_656 . ?
OW1 Zn2 N1 91.3(6) . . ?
OW1 Zn2 N1 88.7(6) 2_656 . ?
N1 Zn2 N1 180.000(1) 2_656 . ?
C5 N1 C1 119.1(12) . . ?
C5 N1 Zn2 121.7(11) . . ?
C1 N1 Zn2 119.1(8) . . ?
C6 N2 C10 121.9(13) . . ?
N1 C1 C2 121.7(14) . . ?
C1 C2 C3 119.8(16) . . ?
C4 C3 C2 115.9(13) . . ?
C4 C3 C8 124.1(13) . . ?
C2 C3 C8 119.8(14) . . ?
C3 C4 C5 120.3(13) . . ?
N1 C5 C4 122.8(15) . . ?
N2 C6 C7 118.2(14) . . ?
C8 C7 C6 122.2(14) . . ?
C7 C8 C9 118.0(14) . . ?
C7 C8 C3 123.0(13) . . ?
C9 C8 C3 119.0(14) . . ?
C10 C9 C8 118.7(17) . . ?
C9 C10 N2 120.7(16) . . ?
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
Mo1 O9 1.712(9) . ?
Mo1 O10 1.722(10) . ?
Mo1 O7 1.917(9) . ?
Mo1 O14 1.955(9) 2 ?
Mo1 O2 2.342(9) 2 ?
Mo1 O1 2.337(9) . ?
Mo2 O11 1.714(10) . ?
Mo2 O12 1.698(9) . ?
Mo2 O7 1.923(10) . ?
Mo2 O8 1.920(10) . ?
Mo2 O3 2.330(8) 2 ?
Mo2 O1 2.324(8) . ?
Mo3 O15 1.707(11) . ?
Mo3 O13 1.698(9) . ?
Mo3 O8 1.920(9) . ?
Mo3 O14 1.939(9) . ?
Mo3 O2 2.315(8) . ?
Mo3 O3 2.332(9) 2 ?
As1 O4 1.779(11) . ?
As1 O1 1.793(8) . ?
As1 O5 1.804(9) . ?
As2 O5 1.776(9) . ?
As2 O3 1.778(7) . ?
As2 O6 1.787(10) . ?
As3 O4 1.789(10) . ?
As3 O2 1.776(8) . ?
As3 O6 1.805(9) . ?
Zn1 O1 2.078(8) 2 ?
Zn1 O1 2.078(8) . ?
Zn1 O3 2.077(7) 2 ?
Zn1 O3 2.077(7) . ?
Zn1 O2 2.120(10) . ?
Zn1 O2 2.120(10) 2 ?
O2 Mo1 2.342(9) 2 ?
O3 Mo2 2.330(8) 2 ?
O3 Mo3 2.332(9) 2 ?
O14 Mo1 1.955(9) 2 ?
Zn2 OW2 2.062(14) . ?
Zn2 OW2 2.062(14) 2_656 ?
Zn2 OW1 2.130(17) . ?
Zn2 OW1 2.130(17) 2_656 ?
Zn2 N1 2.148(11) 2_656 ?
Zn2 N1 2.148(11) . ?
N1 C5 1.297(17) . ?
N1 C1 1.36(2) . ?
N2 C6 1.325(17) . ?
N2 C10 1.38(2) . ?
C1 C2 1.37(2) . ?
C2 C3 1.431(19) . ?
C3 C4 1.37(2) . ?
C3 C8 1.452(19) . ?
C4 C5 1.405(19) . ?
C6 C7 1.40(2) . ?
C7 C8 1.35(2) . ?
C8 C9 1.42(2) . ?
C9 C10 1.36(2) . ?
