#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:21:36 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/44/7014469.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_7014469
loop_
_publ_author_name
'Guo, Si-Xuan'
'Xie, Jingli'
'Gilbert-Wilson, Ryan'
'Birkett, Stephen L.'
'Bond, Alan M.'
'Wedd, Anthony G.'
_publ_section_title
;
 Synthesis and redox properties of triarylmethane dye cation salts of
 anions [M6O19]2- (M = Mo, W).
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              356
_journal_page_last               366
_journal_paper_doi               10.1039/c0dt00882f
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C56 H78 Mo6 N12 O25'
_chemical_formula_weight         1894.94
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.625(2)
_cell_length_b                   16.625(2)
_cell_length_c                   21.725(5)
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      1.70
_cell_volume                     5200.1(15)
_computing_cell_refinement       'SMART (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6957
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2850
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.116
_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     131
_refine_ls_number_reflns         2359
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0409
_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)+(0.0650P)²+28.6964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                2307
_reflns_number_total             2359
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00882F.TXT
_cod_data_source_block           jlryan4m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        5200.1(16)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7014469
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.209435(18) 0.641452(19) 0.228738(12) 0.02060(14) Uani 1 1 d . . .
O1 O 0.20886(17) 0.72224(18) 0.16645(11) 0.0257(5) Uani 1 1 d . . .
O2 O 0.3333 0.6667 0.1667 0.0171(10) Uani 1 6 d S . .
O3 O 0.25447(18) 0.56517(19) 0.26631(12) 0.0266(5) Uani 1 1 d . . .
O4 O 0.11713(18) 0.61789(19) 0.27243(12) 0.0291(5) Uani 1 1 d . . .
O5 O 0.0762(2) 0.2389(2) 0.27035(13) 0.0384(6) Uiso 1 1 d . . .
N1 N 0.3499(2) -0.0237(2) 0.24012(17) 0.0323(7) Uani 1 1 d . . .
H1A H 0.3521 -0.0696 0.2214 0.031(11) Uiso 1 1 calc R . .
H1B H 0.2978 -0.0332 0.2570 0.040(13) Uiso 1 1 calc R . .
N2 N 0.2030(2) 0.2215(2) 0.26345(14) 0.0293(6) Uiso 1 1 d . . .
C1 C 0.6667 0.3333 0.2463(2) 0.0181(10) Uani 1 3 d S . .
C2 C 0.5860(2) 0.2413(2) 0.24571(13) 0.0171(6) Uani 1 1 d . . .
C3 C 0.5008(2) 0.2227(2) 0.27300(14) 0.0190(6) Uani 1 1 d . . .
H3 H 0.4969 0.2721 0.2920 0.025(10) Uiso 1 1 calc R . .
C4 C 0.4240(2) 0.1354(2) 0.27274(15) 0.0215(6) Uani 1 1 d . . .
H4 H 0.3688 0.1249 0.2928 0.018(9) Uiso 1 1 calc R . .
C5 C 0.4264(2) 0.0609(2) 0.24285(15) 0.0222(6) Uani 1 1 d . . .
C6 C 0.5112(2) 0.0781(2) 0.21602(15) 0.0219(6) Uani 1 1 d . . .
H6 H 0.5150 0.0288 0.1967 0.018(9) Uiso 1 1 calc R . .
C7 C 0.5878(2) 0.1653(2) 0.21775(14) 0.0199(6) Uani 1 1 d . . .
H7 H 0.6439 0.1750 0.1996 0.017(9) Uiso 1 1 calc R . .
C8 C 0.3035(4) 0.2667(4) 0.2611(2) 0.0476(11) Uiso 1 1 d . . .
H8A H 0.3302 0.3338 0.2663 0.071 Uiso 1 1 calc R . .
H8B H 0.3227 0.2542 0.2212 0.071 Uiso 1 1 calc R . .
H8C H 0.3256 0.2425 0.2941 0.071 Uiso 1 1 calc R . .
C9 C 0.1511(3) 0.1216(3) 0.25652(18) 0.0350(8) Uiso 1 1 d . . .
H9A H 0.0844 0.0999 0.2588 0.053 Uiso 1 1 calc R . .
H9B H 0.1682 0.0928 0.2895 0.053 Uiso 1 1 calc R . .
H9C H 0.1654 0.1045 0.2165 0.053 Uiso 1 1 calc R . .
C10 C 0.1607(3) 0.2710(3) 0.26970(16) 0.0306(7) Uiso 1 1 d . . .
H10A H 0.1989 0.3363 0.2740 0.037 Uiso 1 1 calc R . .
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'
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
O4 Mo1 O3 105.15(13) . 3_565 ?
O4 Mo1 O1 103.86(12) . . ?
O3 Mo1 O1 88.72(12) 3_565 . ?
O4 Mo1 O3 102.47(12) . . ?
O3 Mo1 O3 87.63(17) 3_565 . ?
O1 Mo1 O3 153.45(11) . . ?
O4 Mo1 O1 101.30(12) . 15 ?
O3 Mo1 O1 153.49(11) 3_565 15 ?
O1 Mo1 O1 86.49(3) . 15 ?
O3 Mo1 O1 85.16(11) . 15 ?
O4 Mo1 O2 177.23(10) . . ?
O3 Mo1 O2 77.40(8) 3_565 . ?
O1 Mo1 O2 77.12(7) . . ?
O3 Mo1 O2 76.42(7) . . ?
O1 Mo1 O2 76.12(7) 15 . ?
Mo1 O1 Mo1 116.26(12) . 14_455 ?
Mo1 O2 Mo1 89.567(14) 13_565 15 ?
Mo1 O2 Mo1 90.435(14) 13_565 3_565 ?
Mo1 O2 Mo1 180.0 15 3_565 ?
Mo1 O2 Mo1 179.999(9) 13_565 . ?
Mo1 O2 Mo1 90.434(14) 15 . ?
Mo1 O2 Mo1 89.564(14) 3_565 . ?
Mo1 O2 Mo1 90.437(14) 13_565 2_665 ?
Mo1 O2 Mo1 90.437(14) 15 2_665 ?
Mo1 O2 Mo1 89.564(14) 3_565 2_665 ?
Mo1 O2 Mo1 89.564(14) . 2_665 ?
Mo1 O2 Mo1 89.565(14) 13_565 14_455 ?
Mo1 O2 Mo1 89.564(14) 15 14_455 ?
Mo1 O2 Mo1 90.435(14) 3_565 14_455 ?
Mo1 O2 Mo1 90.434(14) . 14_455 ?
Mo1 O2 Mo1 180.0 2_665 14_455 ?
Mo1 O3 Mo1 116.61(13) 2_665 . ?
C5 N1 H1A 120.0 . . ?
C5 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C10 N2 C9 121.6(3) . . ?
C10 N2 C8 120.8(4) . . ?
C9 N2 C8 117.5(4) . . ?
C2 C1 C2 119.993(8) 2_655 . ?
C2 C1 C2 119.993(8) 2_655 3_665 ?
C2 C1 C2 119.993(8) . 3_665 ?
C7 C2 C3 116.7(3) . . ?
C7 C2 C1 121.8(3) . . ?
C3 C2 C1 121.6(3) . . ?
C4 C3 C2 121.9(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 120.6(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C6 121.2(3) . . ?
N1 C5 C4 120.7(3) . . ?
C6 C5 C4 118.2(3) . . ?
C7 C6 C5 120.5(3) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C2 122.2(3) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C10 N2 125.2(4) . . ?
O5 C10 H10A 117.4 . . ?
N2 C10 H10A 117.4 . . ?
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 O4 1.676(3) . ?
Mo1 O3 1.893(3) 3_565 ?
Mo1 O1 1.910(2) . ?
Mo1 O3 1.945(3) . ?
Mo1 O1 1.965(2) 15 ?
Mo1 O2 2.3181(4) . ?
O1 Mo1 1.965(2) 14_455 ?
O2 Mo1 2.3180(4) 13_565 ?
O2 Mo1 2.3180(4) 15 ?
O2 Mo1 2.3181(4) 3_565 ?
O2 Mo1 2.3181(4) 2_665 ?
O2 Mo1 2.3181(4) 14_455 ?
O3 Mo1 1.893(2) 2_665 ?
O5 C10 1.229(5) . ?
N1 C5 1.345(4) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N2 C10 1.329(5) . ?
N2 C9 1.446(5) . ?
N2 C8 1.452(6) . ?
C1 C2 1.445(3) 2_655 ?
C1 C2 1.445(3) . ?
C1 C2 1.445(3) 3_665 ?
C2 C7 1.416(4) . ?
C2 C3 1.420(4) . ?
C3 C4 1.372(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.417(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.416(5) . ?
C6 C7 1.370(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9500 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139155843
