#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:22:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179107 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/69/4306931.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_4306931
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            'C30 H38 As2 Mo6 N6 O30'
_chemical_formula_weight         1688.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.691(3)
_cell_length_b                   18.645(4)
_cell_length_c                   10.623(2)
_cell_measurement_reflns_used    9520
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.26
_cell_volume                     2307.9(12)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9520
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.111
_exptl_absorpt_correction_T_max  0.418
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.738
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0247
_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)+(0.0254P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                2298
_reflns_number_total             2704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061227jsi20061203_101348.cif
_cod_data_source_block           s27e
_cod_original_cell_volume        2307.9(8)
_cod_database_code               4306931
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.5000 0.174578(18) 1.5000 0.01601(9) Uani 1 2 d S . .
Mo2 Mo 0.256842(19) 0.088246(13) 1.32453(3) 0.01582(7) Uani 1 1 d . . .
As1 As 0.48392(3) 0.0000 1.32880(4) 0.01075(9) Uani 1 2 d S . .
O1 O 0.45893(18) 0.23095(12) 1.5843(2) 0.0285(5) Uani 1 1 d . . .
OW1 O 0.4721(2) 0.33473(15) 1.1703(4) 0.0349(6) Uani 1 1 d . . .
HW1A H 0.529(3) 0.335(2) 1.239(5) 0.033(12) Uiso 1 1 d . . .
HW1B H 0.463(4) 0.357(2) 1.096(5) 0.046(12) Uiso 1 1 d . . .
O2 O 0.21689(18) 0.14497(12) 1.4098(2) 0.0270(5) Uani 1 1 d . . .
O3 O 0.14233(17) 0.08839(12) 1.1277(2) 0.0236(5) Uani 1 1 d . . .
O4 O 0.2344(2) 0.0000 1.3906(3) 0.0182(6) Uani 1 2 d S . .
O5 O 0.4702(2) 0.0000 1.1576(3) 0.0194(6) Uani 1 2 d S . .
O6 O 0.44182(15) 0.07490(10) 1.5690(2) 0.0149(4) Uani 1 1 d . . .
O7 O 0.35488(16) 0.14838(10) 1.3103(2) 0.0169(4) Uani 1 1 d . . .
O8 O 0.3504(2) 0.0000 1.2789(3) 0.0139(5) Uani 1 2 d S . .
N1 N 0.2922(2) 0.32125(14) 1.1794(3) 0.0222(5) Uani 1 1 d . . .
H1B H 0.3643 0.3206 1.2231 0.027 Uiso 1 1 calc R . .
N2 N 0.2636(3) 0.0000 0.8886(4) 0.0211(7) Uani 1 2 d S . .
H2 H 0.3277 0.0000 0.9827 0.021 Uiso 1 2 calc SR . .
C1 C 0.1021(2) 0.33284(16) 0.9495(3) 0.0209(6) Uani 1 1 d . . .
H1A H 0.0503 0.3404 0.8406 0.025 Uiso 1 1 calc R . .
C2 C 0.2172(3) 0.33239(17) 1.0230(3) 0.0237(6) Uani 1 1 d . . .
H2A H 0.2437 0.3399 0.9638 0.028 Uiso 1 1 calc R . .
C3 C 0.2583(3) 0.31108(18) 1.2707(4) 0.0259(7) Uani 1 1 d . . .
H3A H 0.3124 0.3039 1.3794 0.031 Uiso 1 1 calc R . .
C4 C 0.1430(2) 0.31135(17) 1.2023(3) 0.0235(6) Uani 1 1 d . . .
H4A H 0.1189 0.3045 1.2646 0.028 Uiso 1 1 calc R . .
C5 C 0.0626(2) 0.32190(14) 1.0392(3) 0.0173(6) Uani 1 1 d . . .
C6 C 0.1634(4) 0.0000 0.8655(5) 0.0229(9) Uani 1 2 d S . .
H6A H 0.1642 0.0000 0.9538 0.028 Uiso 1 2 calc SR . .
C7 C 0.0593(3) 0.0000 0.7174(5) 0.0218(9) Uani 1 2 d S . .
H7A H -0.0084 0.0000 0.7067 0.026 Uiso 1 2 calc SR . .
C8 C 0.0554(3) 0.0000 0.5817(4) 0.0171(8) Uani 1 2 d S . .
C9 C 0.1604(3) 0.0000 0.6076(5) 0.0280(10) Uani 1 2 d S . .
H9A H 0.1625 0.0000 0.5219 0.034 Uiso 1 2 calc SR . .
C10 C 0.2609(4) 0.0000 0.7599(5) 0.0279(10) Uani 1 2 d S . .
H10A H 0.3301 0.0000 0.7745 0.033 Uiso 1 2 calc SR . .
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'
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
O1 Mo1 O1 104.21(16) 2_658 . ?
O1 Mo1 O7 97.37(9) 2_658 . ?
O1 Mo1 O7 100.81(9) . . ?
O1 Mo1 O7 100.81(9) 2_658 2_658 ?
O1 Mo1 O7 97.37(9) . 2_658 ?
O7 Mo1 O7 150.21(12) . 2_658 ?
O1 Mo1 O6 90.66(9) 2_658 2_658 ?
O1 Mo1 O6 164.44(9) . 2_658 ?
O7 Mo1 O6 81.46(7) . 2_658 ?
O7 Mo1 O6 74.96(7) 2_658 2_658 ?
O1 Mo1 O6 164.44(9) 2_658 . ?
O1 Mo1 O6 90.66(9) . . ?
O7 Mo1 O6 74.96(7) . . ?
O7 Mo1 O6 81.46(7) 2_658 . ?
O6 Mo1 O6 74.96(9) 2_658 . ?
O3 Mo2 O2 104.31(10) . . ?
O3 Mo2 O4 101.01(11) . . ?
O2 Mo2 O4 98.48(10) . . ?
O3 Mo2 O7 97.50(9) . . ?
O2 Mo2 O7 101.43(10) . . ?
O4 Mo2 O7 148.44(9) . . ?
O3 Mo2 O6 163.87(8) . . ?
O2 Mo2 O6 91.09(9) . . ?
O4 Mo2 O6 81.06(9) . . ?
O7 Mo2 O6 74.35(7) . . ?
O3 Mo2 O8 90.69(9) . . ?
O2 Mo2 O8 164.43(9) . . ?
O4 Mo2 O8 74.16(8) . . ?
O7 Mo2 O8 80.32(7) . . ?
O6 Mo2 O8 74.38(8) . . ?
O8 As1 O6 111.82(8) . 2_658 ?
O8 As1 O6 111.82(8) . 5_658 ?
O6 As1 O6 110.86(13) 2_658 5_658 ?
O8 As1 O5 107.72(13) . . ?
O6 As1 O5 107.17(8) 2_658 . ?
O6 As1 O5 107.17(8) 5_658 . ?
HW1A OW1 HW1B 113(4) . . ?
Mo2 O4 Mo2 120.53(13) 6 . ?
As1 O6 Mo1 129.69(9) 5_658 . ?
As1 O6 Mo2 130.58(10) 5_658 . ?
Mo1 O6 Mo2 88.11(6) . . ?
Mo1 O7 Mo2 118.78(9) . . ?
As1 O8 Mo2 129.83(7) . 6 ?
As1 O8 Mo2 129.83(7) . . ?
Mo2 O8 Mo2 87.69(8) 6 . ?
C2 N1 C3 122.1(3) . . ?
C2 N1 H1B 119.0 . . ?
C3 N1 H1B 119.0 . . ?
C6 N2 C10 117.8(4) . . ?
C6 N2 H2 121.1 . . ?
C10 N2 H2 121.1 . . ?
C2 C1 C5 119.6(3) . . ?
C2 C1 H1A 120.2 . . ?
C5 C1 H1A 120.2 . . ?
N1 C2 C1 120.5(3) . . ?
N1 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
N1 C3 C4 119.6(3) . . ?
N1 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C4 C5 C1 118.5(3) . . ?
C4 C5 C5 121.2(3) . 2_557 ?
C1 C5 C5 120.2(3) . 2_557 ?
N2 C6 C7 122.9(4) . . ?
N2 C6 H6A 118.6 . . ?
C7 C6 H6A 118.6 . . ?
C6 C7 C8 119.8(4) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C9 C8 C7 116.6(4) . . ?
C9 C8 C8 121.6(4) . 5_556 ?
C7 C8 C8 121.8(4) . 5_556 ?
C10 C9 C8 120.0(4) . . ?
C10 C9 H9A 120.0 . . ?
C8 C9 H9A 120.0 . . ?
N2 C10 C9 122.9(4) . . ?
N2 C10 H10A 118.6 . . ?
C9 C10 H10A 118.6 . . ?
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 O1 1.711(2) 2_658 ?
Mo1 O1 1.711(2) . ?
Mo1 O7 1.901(2) . ?
Mo1 O7 1.901(2) 2_658 ?
Mo1 O6 2.3421(19) 2_658 ?
Mo1 O6 2.3421(19) . ?
Mo2 O3 1.708(2) . ?
Mo2 O2 1.712(2) . ?
Mo2 O4 1.8949(13) . ?
Mo2 O7 1.903(2) . ?
Mo2 O6 2.365(2) . ?
Mo2 O8 2.3754(18) . ?
As1 O8 1.692(2) . ?
As1 O6 1.6959(19) 2_658 ?
As1 O6 1.6959(19) 5_658 ?
As1 O5 1.703(2) . ?
OW1 HW1A 0.70(4) . ?
OW1 HW1B 0.83(5) . ?
O4 Mo2 1.8949(13) 6 ?
O6 As1 1.6959(19) 5_658 ?
O8 Mo2 2.3754(18) 6 ?
N1 C2 1.338(4) . ?
N1 C3 1.347(4) . ?
N1 H1B 0.8600 . ?
N2 C6 1.338(5) . ?
N2 C10 1.343(5) . ?
N2 H2 0.8600 . ?
C1 C2 1.363(4) . ?
C1 C5 1.400(4) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C4 1.377(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.394(4) . ?
C4 H4A 0.9300 . ?
C5 C5 1.487(5) 2_557 ?
C6 C7 1.372(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.408(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.391(5) . ?
C8 C8 1.491(7) 5_556 ?
C9 C10 1.374(6) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
