#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:43:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301803 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/37/2203765.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_2203765
loop_
_publ_author_name
'Shu-Mei Chen'
'Can-Zhong Lu'
'Ya-Qin Yu'
'Quan-Zheng Zhang'
'Xiang He'
_publ_section_title
;
 Bis(tetramethylammonium) hexaaquacobalt(II) β-octamolybdate(VI)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m723
_journal_page_last               m725
_journal_paper_doi               10.1107/S1600536804007524
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '(C4 H12 N)2 [Co (H2 O)6] [Mo8 O26]'
_chemical_formula_moiety         'Mo8 O26 4-, Co H12 O6 2+, 2C4 H12 N 1+'
_chemical_formula_sum            'C8 H36 Co Mo8 N2 O32'
_chemical_formula_weight         1498.84
_chemical_name_systematic
;
Bis(tetramethylammonium) hexaaquacobalt(II) β-octamolybdate(vi)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.7790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0338(10)
_cell_length_b                   13.6400(8)
_cell_length_c                   16.6764(10)
_cell_measurement_reflns_used    3856
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      1.97
_cell_volume                     3621.6(4)
_computing_cell_refinement       'SMART and SAINT (Siemens,1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP in SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5426
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.225
_exptl_absorpt_correction_T_max  .525
_exptl_absorpt_correction_T_min  .421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.680
_refine_diff_density_min         -1.020
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0357P)²+82.4908P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                2825
_reflns_number_total             3195
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg6029.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2203765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Mo1 0.25091(4) 0.83709(4) 0.42069(4) 0.02126(17) Uani d . 1 Mo
Mo2 0.39635(4) 0.85422(5) 0.57132(4) 0.02574(18) Uani d . 1 Mo
Mo3 0.10500(4) 0.85708(5) 0.53760(4) 0.02534(18) Uani d . 1 Mo
Mo4 0.25069(4) 0.87542(5) 0.69005(4) 0.02813(18) Uani d . 1 Mo
Co1 0.2500 1.2500 0.5000 0.0247(3) Uani d S 1 Co
OW1 0.2267(4) 1.1894(5) 0.6112(4) 0.0419(14) Uani d . 1 O
HW1A 0.2385 1.1309 0.6121 0.10(5) Uiso calc R 1 H
HW1B 0.2196 1.2307 0.6454 0.13(7) Uiso d R 1 H
O1 0.5009(3) 0.8290(5) 0.5876(4) 0.0400(14) Uani d . 1 O
OW2 0.3282(3) 1.3546(4) 0.5599(3) 0.0329(12) Uani d . 1 O
HW2A 0.2997 1.3954 0.5804 0.06(3) Uiso calc R 1 H
HW2B 0.3659 1.3802 0.5383 0.05(3) Uiso d R 1 H
O2 0.2503(3) 0.7921(4) 0.3226(3) 0.0288(11) Uani d . 1 O
OW3 0.1489(4) 1.3403(4) 0.5117(4) 0.0413(15) Uani d . 1 O
HW3B 0.1545 1.3919 0.4877 0.14(7) Uiso calc R 1 H
HW3A 0.1108 1.3271 0.5386 0.07(4) Uiso d R 1 H
O3 0.1108(4) 0.9798(4) 0.5207(4) 0.0381(13) Uani d . 1 O
O4 0.2506(4) 0.8613(4) 0.7913(4) 0.0451(15) Uani d . 1 O
O5 0.0007(3) 0.8312(5) 0.5291(4) 0.0431(15) Uani d . 1 O
O6 0.3906(4) 0.9770(4) 0.5537(3) 0.0387(14) Uani d . 1 O
O7 0.2499(3) 0.6687(4) 0.4499(3) 0.0245(11) Uani d . 1 O
O8 0.1344(3) 0.8506(4) 0.6511(3) 0.0314(12) Uani d . 1 O
O9 0.1320(3) 0.8131(4) 0.4291(3) 0.0244(11) Uani d . 1 O
O10 0.3690(3) 0.8117(4) 0.4570(3) 0.0259(11) Uani d . 1 O
O11 0.2514(4) 0.9986(4) 0.6746(4) 0.0421(14) Uani d . 1 O
O12 0.3661(3) 0.8478(4) 0.6769(3) 0.0283(11) Uani d . 1 O
O13 0.2502(3) 0.9597(4) 0.4103(3) 0.0306(12) Uani d . 1 O
N1 0.5000 1.1287(7) 0.7500 0.034(2) Uani d S 1 N
N2 0.0000 0.9396(7) 0.2500 0.030(2) Uani d S 1 N
C1 0.4479(9) 1.1910(13) 0.6923(9) 0.105(6) Uani d . 1 C
H1A 0.4130 1.2323 0.7210 0.157 Uiso calc R 1 H
H1B 0.4132 1.1505 0.6550 0.157 Uiso calc R 1 H
H1C 0.4835 1.2310 0.6633 0.157 Uiso calc R 1 H
C2 0.5554(8) 1.0666(11) 0.7059(9) 0.086(4) Uani d . 1 C
H2A 0.5890 1.0253 0.7435 0.130 Uiso calc R 1 H
H2B 0.5914 1.1077 0.6783 0.130 Uiso calc R 1 H
H2C 0.5217 1.0267 0.6673 0.130 Uiso calc R 1 H
C3 0.0569(7) 0.8774(9) 0.2072(7) 0.065(3) Uani d . 1 C
H3A 0.0241 0.8370 0.1683 0.098 Uiso calc R 1 H
H3B 0.0901 0.8366 0.2456 0.098 Uiso calc R 1 H
H3C 0.0933 0.9186 0.1802 0.098 Uiso calc R 1 H
C4 0.0514(6) 1.0029(7) 0.3098(5) 0.044(2) Uani d . 1 C
H4A 0.0149 1.0434 0.3373 0.066 Uiso calc R 1 H
H4B 0.0876 1.0437 0.2822 0.066 Uiso calc R 1 H
H4C 0.0847 0.9624 0.3483 0.066 Uiso calc R 1 H
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'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O13 Mo1 O2 . . 104.7(3) yes
O13 Mo1 O10 . . 101.7(2) yes
O2 Mo1 O10 . . 97.2(2) yes
O13 Mo1 O9 . . 100.3(2) yes
O2 Mo1 O9 . . 96.4(2) yes
O10 Mo1 O9 . . 150.2(2) yes
O13 Mo1 O7 . 7_566 98.0(2) yes
O2 Mo1 O7 . 7_566 157.3(2) yes
O10 Mo1 O7 . 7_566 78.67(19) yes
O9 Mo1 O7 . 7_566 78.57(19) yes
O13 Mo1 O7 . . 173.8(2) yes
O2 Mo1 O7 . . 81.4(2) yes
O10 Mo1 O7 . . 78.01(19) yes
O9 Mo1 O7 . . 77.93(18) yes
O7 Mo1 O7 7_566 . 75.9(2) yes
O1 Mo2 O6 . . 105.0(3) yes
O1 Mo2 O12 . . 101.5(3) yes
O6 Mo2 O12 . . 101.1(3) yes
O1 Mo2 O10 . . 101.2(3) yes
O6 Mo2 O10 . . 96.9(2) yes
O12 Mo2 O10 . . 146.1(2) yes
O1 Mo2 O9 . 7_566 89.5(2) yes
O6 Mo2 O9 . 7_566 163.4(2) yes
O12 Mo2 O9 . 7_566 83.4(2) yes
O10 Mo2 O9 . 7_566 71.99(19) yes
O1 Mo2 O7 . 7_566 160.7(2) yes
O6 Mo2 O7 . 7_566 94.1(2) yes
O12 Mo2 O7 . 7_566 76.8(2) yes
O10 Mo2 O7 . 7_566 73.42(18) yes
O9 Mo2 O7 7_566 7_566 71.21(16) yes
O5 Mo3 O3 . . 105.3(3) yes
O5 Mo3 O8 . . 101.5(3) yes
O3 Mo3 O8 . . 101.5(3) yes
O5 Mo3 O9 . . 100.3(3) yes
O3 Mo3 O9 . . 97.1(2) yes
O8 Mo3 O9 . . 146.4(2) yes
O5 Mo3 O7 . 7_566 159.4(2) yes
O3 Mo3 O7 . 7_566 95.1(2) yes
O8 Mo3 O7 . 7_566 77.1(2) yes
O9 Mo3 O7 . 7_566 73.54(18) yes
O5 Mo3 O10 . 7_566 88.2(2) yes
O3 Mo3 O10 . 7_566 164.0(2) yes
O8 Mo3 O10 . 7_566 83.9(2) yes
O9 Mo3 O10 . 7_566 71.56(18) yes
O7 Mo3 O10 7_566 7_566 71.20(17) yes
O4 Mo4 O11 . . 105.2(3) yes
O4 Mo4 O12 . . 101.8(3) yes
O11 Mo4 O12 . . 98.7(3) yes
O4 Mo4 O8 . . 101.6(3) yes
O11 Mo4 O8 . . 98.4(3) yes
O12 Mo4 O8 . . 146.1(2) yes
O4 Mo4 O2 . 7_566 88.7(2) yes
O11 Mo4 O2 . 7_566 166.0(2) yes
O12 Mo4 O2 . 7_566 78.0(2) yes
O8 Mo4 O2 . 7_566 78.4(2) yes
O4 Mo4 O7 . 7_566 159.0(2) yes
O11 Mo4 O7 . 7_566 95.7(2) yes
O12 Mo4 O7 . 7_566 74.59(19) yes
O8 Mo4 O7 . 7_566 74.78(19) yes
O2 Mo4 O7 7_566 7_566 70.28(17) yes
OW3 Co1 OW3 7_576 . 180.000(2) yes
OW3 Co1 OW2 7_576 7_576 88.9(2) yes
OW3 Co1 OW2 . 7_576 91.1(2) yes
OW3 Co1 OW2 7_576 . 91.1(2) yes
OW3 Co1 OW2 . . 88.9(2) yes
OW2 Co1 OW2 7_576 . 180.0000(10) yes
OW3 Co1 OW1 7_576 . 94.1(3) yes
OW3 Co1 OW1 . . 85.9(3) yes
OW2 Co1 OW1 7_576 . 89.7(2) yes
OW2 Co1 OW1 . . 90.3(2) yes
OW3 Co1 OW1 7_576 7_576 85.9(3) yes
OW3 Co1 OW1 . 7_576 94.1(3) yes
OW2 Co1 OW1 7_576 7_576 90.3(2) yes
OW2 Co1 OW1 . 7_576 89.7(2) yes
OW1 Co1 OW1 . 7_576 180.0000(10) yes
Co1 OW1 HW1A . . 109.5 no
Co1 OW1 HW1B . . 113.4 no
HW1A OW1 HW1B . . 135.1 no
Co1 OW2 HW2A . . 109.5 no
Co1 OW2 HW2B . . 121.1 no
HW2A OW2 HW2B . . 111.8 no
Mo1 O2 Mo4 . 7_566 115.8(2) no
Co1 OW3 HW3B . . 109.5 no
Co1 OW3 HW3A . . 124.4 no
HW3B OW3 HW3A . . 126.0 no
Mo1 O7 Mo3 7_566 7_566 91.61(18) no
Mo1 O7 Mo1 7_566 . 104.1(2) no
Mo3 O7 Mo1 7_566 . 97.73(18) no
Mo1 O7 Mo2 7_566 7_566 91.26(17) no
Mo3 O7 Mo2 7_566 7_566 163.3(2) no
Mo1 O7 Mo2 . 7_566 97.50(18) no
Mo1 O7 Mo4 7_566 7_566 163.4(2) no
Mo3 O7 Mo4 7_566 7_566 86.50(16) no
Mo1 O7 Mo4 . 7_566 92.47(17) no
Mo2 O7 Mo4 7_566 7_566 86.07(16) no
Mo3 O8 Mo4 . . 116.3(3) no
Mo1 O9 Mo3 . . 109.3(2) no
Mo1 O9 Mo2 . 7_566 110.8(2) no
Mo3 O9 Mo2 . 7_566 103.5(2) no
Mo1 O10 Mo2 . . 109.9(2) no
Mo1 O10 Mo3 . 7_566 110.4(2) no
Mo2 O10 Mo3 . 7_566 103.4(2) no
Mo2 O12 Mo4 . . 117.1(3) no
C1 N1 C1 2_656 . 109.2(16) no
C1 N1 C2 2_656 2_656 109.4(9) no
C1 N1 C2 . 2_656 109.1(9) no
C1 N1 C2 2_656 . 109.1(9) no
C1 N1 C2 . . 109.4(9) no
C2 N1 C2 2_656 . 110.5(13) no
C3 N2 C3 . 2 110.5(12) no
C3 N2 C4 . . 109.2(6) no
C3 N2 C4 2 . 109.3(6) no
C3 N2 C4 . 2 109.3(6) no
C3 N2 C4 2 2 109.2(6) no
C4 N2 C4 . 2 109.2(9) no
N1 C1 H1A . . 109.5 no
N1 C1 H1B . . 109.5 no
H1A C1 H1B . . 109.5 no
N1 C1 H1C . . 109.5 no
H1A C1 H1C . . 109.5 no
H1B C1 H1C . . 109.5 no
N1 C2 H2A . . 109.5 no
N1 C2 H2B . . 109.5 no
H2A C2 H2B . . 109.5 no
N1 C2 H2C . . 109.5 no
H2A C2 H2C . . 109.5 no
H2B C2 H2C . . 109.5 no
N2 C3 H3A . . 109.5 no
N2 C3 H3B . . 109.5 no
H3A C3 H3B . . 109.5 no
N2 C3 H3C . . 109.5 no
H3A C3 H3C . . 109.5 no
H3B C3 H3C . . 109.5 no
N2 C4 H4A . . 109.5 no
N2 C4 H4B . . 109.5 no
H4A C4 H4B . . 109.5 no
N2 C4 H4C . . 109.5 no
H4A C4 H4C . . 109.5 no
H4B C4 H4C . . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 O13 . 1.681(5) yes
Mo1 O2 . 1.746(5) yes
Mo1 O10 . 1.950(5) yes
Mo1 O9 . 1.956(5) yes
Mo1 O7 7_566 2.162(5) yes
Mo1 O7 . 2.348(5) yes
Mo2 O1 . 1.701(5) yes
Mo2 O6 . 1.701(5) yes
Mo2 O12 . 1.882(5) yes
Mo2 O10 . 1.992(5) yes
Mo2 O9 7_566 2.327(5) yes
Mo2 O7 7_566 2.350(5) yes
Mo3 O5 . 1.699(6) yes
Mo3 O3 . 1.701(5) yes
Mo3 O8 . 1.898(5) yes
Mo3 O9 . 2.002(5) yes
Mo3 O7 7_566 2.338(5) yes
Mo3 O10 7_566 2.339(5) yes
Mo4 O4 . 1.699(6) yes
Mo4 O11 . 1.700(6) yes
Mo4 O12 . 1.926(5) yes
Mo4 O8 . 1.931(6) yes
Mo4 O2 7_566 2.295(5) yes
Mo4 O7 7_566 2.409(5) yes
Co1 OW3 7_576 2.063(5) no
Co1 OW3 . 2.063(5) yes
Co1 OW2 7_576 2.076(5) no
Co1 OW2 . 2.076(5) yes
Co1 OW1 . 2.104(6) yes
Co1 OW1 7_576 2.104(6) no
OW1 HW1A . 0.8200 no
OW1 HW1B . 0.8200 no
OW2 HW2A . 0.8200 no
OW2 HW2B . 0.8184 no
O2 Mo4 7_566 2.295(5) no
OW3 HW3B . 0.8200 no
OW3 HW3A . 0.8191 no
O7 Mo1 7_566 2.162(5) no
O7 Mo3 7_566 2.338(5) no
O7 Mo2 7_566 2.350(5) no
O7 Mo4 7_566 2.409(5) no
O9 Mo2 7_566 2.327(5) no
O10 Mo3 7_566 2.339(5) no
N1 C1 2_656 1.469(12) no
N1 C1 . 1.469(12) no
N1 C2 2_656 1.483(12) no
N1 C2 . 1.483(12) no
N2 C3 . 1.488(11) no
N2 C3 2 1.488(11) no
N2 C4 . 1.492(10) no
N2 C4 2 1.492(10) no
C1 H1A . 0.9600 no
C1 H1B . 0.9600 no
C1 H1C . 0.9600 no
C2 H2A . 0.9600 no
C2 H2B . 0.9600 no
C2 H2C . 0.9600 no
C3 H3A . 0.9600 no
C3 H3B . 0.9600 no
C3 H3C . 0.9600 no
C4 H4A . 0.9600 no
C4 H4B . 0.9600 no
C4 H4C . 0.9600 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
OW1 HW1A O11 . 0.82 2.08 2.819(8) 150
OW1 HW1B O4 4_556 0.82 2.10 2.852(9) 153
OW2 HW2A O13 7_576 0.82 2.14 2.897(7) 152
OW2 HW2A O4 4_556 0.82 2.42 2.916(8) 120
OW2 HW2B O3 7_576 0.82 2.20 2.859(8) 138
OW2 HW2B O5 3 0.82 2.28 2.889(8) 131
OW3 HW3B O6 7_576 0.82 2.02 2.764(8) 151
OW3 HW3A O1 3_455 0.82 2.03 2.822(8) 163
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168308745
