#------------------------------------------------------------------------------
#$Date: 2017-07-11 19:31:59 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198643 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/12/2001201.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2001201
loop_
_publ_author_name
'Harrison, W. T. A.'
'Stucky, G. D.'
'Gier, T. E.'
_publ_section_title
;
 Tetrakis(tetramethylammonium) octamolybdate dihydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1900
_journal_page_last               1902
_journal_paper_doi               10.1107/S0108270193004810
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         '[N1 (C1 H3 )4 ]4 '[Mo8 O26]. 2H2 O1'
_chemical_formula_structural     '[N(CH~3~)~4~]~4~.Mo~8~O~26~.2H~2~O'
_chemical_formula_sum            'C16 H52 Mo8 N4 O28'
_chemical_formula_weight         1516.12
_chemical_name_systematic
;
Tetra-(tetramethylammonium) Octamolybdate Dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.301(6)
_cell_angle_beta                 108.962(5)
_cell_angle_gamma                75.234(4)
_cell_formula_units_Z            1
_cell_length_a                   10.539(2)
_cell_length_b                   11.902(2)
_cell_length_c                   9.714(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      9
_cell_measurement_theta_min      5
_cell_volume                     1113.8(4)
_computing_cell_refinement       'UCLA Crystallographic Software'
_computing_data_collection
'UCLA crystallographic software (Strouse, 1982)'
_computing_data_reduction        'UCLA Crystallographic Software'
_computing_molecular_graphics    'locally modified ORTEPII (Johnson, 1976)'
_computing_publication_material  'local routines'
_computing_structure_refinement
'CRYSTALS (Carruthers, Watkin & Betteridge, 1990)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       'Huber automated diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2550
_diffrn_reflns_reduction_process 'Lehman-Larsen method'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         0.0
_diffrn_standards_decay_%        <+-2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.22
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_description       lump
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.89
_refine_ls_extinction_coef       42(4)
_refine_ls_extinction_method     Larson
_refine_ls_hydrogen_treatment    'H atom positions not determined'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     218
_refine_ls_number_reflns         1805
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .048
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         .050
_reflns_number_observed          1805
_reflns_number_total             2550
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            hh1072.cif
_cod_data_source_block           TOZ
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-07-11
;
_cod_original_cell_volume        1114(2)
_cod_database_code               2001201
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
_atom_site_attached_hydrogens
Mo(1) 0.97190(10) 0.47840(10) 0.16500(10) 0.0342 Uani ? ? Mo 0
Mo(2) 0.93280(10) 0.25850(10) -0.25280(10) 0.0431 Uani ? ? Mo 0
Mo(3) 1.18280(10) 0.27190(10) 0.05040(10) 0.0360 Uani ? ? Mo 0
Mo(4) 0.72390(10) 0.46750(10) -0.13240(10) 0.0378 Uani ? ? Mo 0
O(1) 0.9643(9) 0.3934(7) -0.0430(10) 0.0369 Uani ? ? O 0
O(2) 0.9265(9) 0.3811(8) 0.2380(10) 0.0444 Uani ? ? O 0
O(3) 1.1662(8) 0.4046(7) 0.1922(9) 0.0313 Uani ? ? O 0
O(4) 0.7922(9) 0.5649(7) 0.0436(9) 0.0373 Uani ? ? O 0
O(5) 0.9965(9) 0.5871(8) 0.3000(10) 0.0453 Uani ? ? O 0
O(6) 0.7662(9) 0.3775(8) -0.2939(9) 0.0409 Uani ? ? O 0
O(7) 1.1305(9) 0.2193(8) -0.1450(10) 0.0422 Uani ? ? O 0
O(8) 0.8840(10) 0.1644(8) -0.1710(10) 0.0541 Uani ? ? O 0
O(9) 0.9330(10) 0.1957(9) -0.4180(10) 0.0642 Uani ? ? O 0
O(10) 1.1300(10) 0.1810(8) 0.1300(10) 0.0463 Uani ? ? O 0
O(11) 1.3590(10) 0.2166(8) 0.0950(10) 0.0542 Uani ? ? O 0
O(12) 0.6870(10) 0.3680(9) -0.0510(10) 0.0545 Uani ? ? O 0
O(13) 0.5690(10) 0.5553(8) -0.2180(10) 0.0520 Uani ? ? O 0
O(20) 0.698(2) 0.0160(10) 0.691(2) 0.1063 Uani ? ? O 2
N(1) 0.7500(10) 0.1180(10) 0.2030(10) 0.0501 Uani ? ? N 0
N(2) 0.6550(10) 0.6830(10) 0.4130(10) 0.0485 Uani ? ? N 0
C(1) 0.691(2) 0.2420(10) 0.246(2) 0.0515 Uani ? ? C 3
C(2) 0.737(2) 0.0350(10) 0.303(2) 0.0696 Uani ? ? C 3
C(3) 0.901(2) 0.105(2) 0.218(2) 0.0655 Uani ? ? C 3
C(4) 0.673(2) 0.095(2) 0.047(2) 0.0767 Uani ? ? C 3
C(5) 0.769(2) 0.745(2) 0.493(2) 0.0620 Uani ? ? C 3
C(6) 0.598(2) 0.723(2) 0.257(2) 0.0633 Uani ? ? C 3
C(7) 0.710(2) 0.5550(10) 0.421(2) 0.0688 Uani ? ? C 3
C(8) 0.544(2) 0.721(2) 0.489(2) 0.0692 Uani ? ? C 3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo ? ? ? International_Tables_Vol_IV_Table_2.2B
O ? ? ? International_Tables_Vol_IV_Table_2.2B
N ? ? ? International_Tables_Vol_IV_Table_2.2B
C ? ? ? International_Tables_Vol_IV_Table_2.2B
H ? ? ? International_Tables_Vol_IV_Table_2.2B
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 -1 0
1 0 2
0 -3 -3
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O(1) Mo(1) O(1) . . 2_765 76.3(3) yes
O(2) Mo(1) O(1) . . . 98.8(4) yes
O(2) Mo(1) O(1) . . 2_765 175.1(4) yes
O(3) Mo(1) O(1) . . . 78.1(3) yes
O(3) Mo(1) O(1) . . 2_765 78.2(3) yes
O(3) Mo(1) O(2) . . . 100.7(4) yes
O(4) Mo(1) O(1) . . . 79.2(3) yes
O(4) Mo(1) O(1) . . 2_765 77.7(3) yes
O(4) Mo(1) O(2) . . . 101.8(4) yes
O(4) Mo(1) O(3) . . . 150.1(4) yes
O(5) Mo(1) O(1) . . . 156.9(4) yes
O(5) Mo(1) O(1) . . 2_765 80.6(4) yes
O(5) Mo(1) O(2) . . . 104.3(4) yes
O(5) Mo(1) O(3) . . . 97.5(4) yes
O(5) Mo(1) O(4) . . . 95.7(4) yes
O(5) Mo(2) O(1) 2_765 . . 69.7(3) yes
O(6) Mo(2) O(1) . . . 74.6(3) yes
O(6) Mo(2) O(5) . . 2_765 78.0(4) yes
O(7) Mo(2) O(1) . . . 74.0(3) yes
O(7) Mo(2) O(5) . . 2_765 78.1(4) yes
O(7) Mo(2) O(6) . . . 145.5(4) yes
O(8) Mo(2) O(1) . . . 94.0(4) yes
O(8) Mo(2) O(5) . . 2_765 163.7(4) yes
O(8) Mo(2) O(6) . . . 98.4(4) yes
O(8) Mo(2) O(7) . . . 97.7(4) yes
O(9) Mo(2) O(1) . . . 161.2(5) yes
O(9) Mo(2) O(5) . . 2_765 91.6(5) yes
O(9) Mo(2) O(6) . . . 103.9(5) yes
O(9) Mo(2) O(7) . . . 101.2(5) yes
O(9) Mo(2) O(8) . . . 104.7(5) yes
O(3) Mo(3) O(1) . . . 73.0(3) yes
O(4) Mo(3) O(1) 2_765 . . 71.7(3) yes
O(4) Mo(3) O(3) 2_765 . . 71.5(3) yes
O(7) Mo(3) O(1) . . . 78.1(3) yes
O(7) Mo(3) O(3) . . . 147.0(3) yes
O(7) Mo(3) O(4) . . 2_765 84.8(4) yes
O(10) Mo(3) O(1) . . . 95.3(4) yes
O(10) Mo(3) O(3) . . . 96.9(4) yes
O(10) Mo(3) O(4) . . 2_765 164.4(4) yes
O(10) Mo(3) O(7) . . . 101.2(4) yes
O(11) Mo(3) O(1) . . . 161.1(4) yes
O(11) Mo(3) O(3) . . . 102.8(4) yes
O(11) Mo(3) O(4) . . 2_765 89.4(4) yes
O(11) Mo(3) O(7) . . . 99.5(5) yes
O(11) Mo(3) O(10) . . . 103.6(5) yes
O(3) Mo(4) O(1) 2_765 . . 71.5(3) yes
O(4) Mo(4) O(1) . . . 73.6(3) yes
O(4) Mo(4) O(3) . . 2_765 71.2(3) yes
O(6) Mo(4) O(1) . . . 76.8(3) yes
O(6) Mo(4) O(3) . . 2_765 83.4(3) yes
O(6) Mo(4) O(4) . . . 145.8(4) yes
O(12) Mo(4) O(1) . . . 94.3(4) yes
O(12) Mo(4) O(3) . . 2_765 164.0(4) yes
O(12) Mo(4) O(4) . . . 98.3(4) yes
O(12) Mo(4) O(6) . . . 100.8(4) yes
O(13) Mo(4) O(1) . . . 160.3(4) yes
O(13) Mo(4) O(3) . . 2_765 88.9(4) yes
O(13) Mo(4) O(4) . . . 101.4(4) yes
O(13) Mo(4) O(6) . . . 100.6(4) yes
O(13) Mo(4) O(12) . . . 105.4(5) yes
Mo(1) O(1) Mo(1) . . 2_765 103.7(3) yes
Mo(2) O(1) Mo(1) . . . 164.1(4) yes
Mo(2) O(1) Mo(1) . . 2_765 92.1(3) yes
Mo(3) O(1) Mo(1) . . . 92.2(3) yes
Mo(3) O(1) Mo(1) . . 2_765 97.6(3) yes
Mo(3) O(1) Mo(2) . . . 86.5(3) yes
Mo(4) O(1) Mo(1) . . . 91.4(3) yes
Mo(4) O(1) Mo(1) . . 2_765 97.1(3) yes
Mo(4) O(1) Mo(2) . . . 85.6(3) yes
Mo(4) O(1) Mo(3) . . . 163.5(4) yes
Mo(3) O(3) Mo(1) . . . 109.9(4) yes
Mo(4) O(3) Mo(1) 2_765 . . 110.5(4) yes
Mo(4) O(3) Mo(3) 2_765 . . 103.9(4) yes
Mo(3) O(4) Mo(1) 2_765 . . 110.4(4) yes
Mo(4) O(4) Mo(1) . . . 109.0(4) yes
Mo(4) O(4) Mo(3) . . 2_765 104.1(4) yes
Mo(2) O(5) Mo(1) 2_765 . . 117.6(5) yes
Mo(4) O(6) Mo(2) . . . 117.2(4) yes
Mo(3) O(7) Mo(2) . . . 116.8(5) yes
C(2) N(1) C(1) . . . 109.2(12) no
C(3) N(1) C(1) . . . 108.7(12) no
C(3) N(1) C(2) . . . 109.7(13) no
C(4) N(1) C(1) . . . 109.1(12) no
C(4) N(1) C(2) . . . 110.8(13) no
C(4) N(1) C(3) . . . 109.3(14) no
C(6) N(2) C(5) . . . 107.4(12) no
C(7) N(2) C(5) . . . 110.6(12) no
C(7) N(2) C(6) . . . 111.9(13) no
C(8) N(2) C(5) . . . 106.9(12) no
C(8) N(2) C(6) . . . 110.2(12) no
C(8) N(2) C(7) . . . 109.8(13) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo(1) O(1) . . 2.142(9) yes
Mo(1) O(1) . 2_765 2.373(9) yes
Mo(1) O(2) . . 1.660(9) yes
Mo(1) O(3) . . 1.950(8) yes
Mo(1) O(4) . . 1.960(8) yes
Mo(1) O(5) . . 1.745(9) yes
Mo(2) O(1) . . 2.440(9) yes
Mo(2) O(5) . 2_765 2.290(10) yes
Mo(2) O(6) . . 1.906(9) yes
Mo(2) O(7) . . 1.958(9) yes
Mo(2) O(8) . . 1.700(10) yes
Mo(2) O(9) . . 1.690(10) yes
Mo(3) O(1) . . 2.330(9) yes
Mo(3) O(3) . . 1.989(8) yes
Mo(3) O(4) . 2_765 2.342(9) yes
Mo(3) O(7) . . 1.881(9) yes
Mo(3) O(10) . . 1.690(10) yes
Mo(3) O(11) . . 1.720(10) yes
Mo(4) O(1) . . 2.351(9) yes
Mo(4) O(3) . 2_765 2.351(9) yes
Mo(4) O(4) . . 1.994(9) yes
Mo(4) O(6) . . 1.908(9) yes
Mo(4) O(12) . . 1.680(10) yes
Mo(4) O(13) . . 1.693(9) yes
N(1) C(1) . . 1.51(2) yes
N(1) C(2) . . 1.52(2) yes
N(1) C(3) . . 1.51(2) yes
N(1) C(4) . . 1.50(2) yes
N(2) C(5) . . 1.52(2) yes
N(2) C(6) . . 1.52(2) yes
N(2) C(7) . . 1.49(2) yes
N(2) C(8) . . 1.53(2) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
