#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:05:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179439 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/36/4333644.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_4333644
loop_
_publ_author_name
'Khadija Hakouk'
'Olivier Oms'
'Anne Dolbecq'
'Hani El Moll'
'Jérôme Marrot'
'Michel Evain'
'Florian Molton'
'Carole Duboc'
'Philippe Deniard'
'Stéphane Jobic'
'Pierre Mialane'
'Rémi Dessapt'
_publ_contact_author_address
;Institut des Materiaux JeanRouxel,
 Universite de Nantes, CNRS, 2 rue de la, Houssiniere, BP 32229,44322 Nantes
;
_publ_contact_author_email       remi.dessapt@cnrs-imn.fr
_publ_contact_author_name        'Dessapt, Remi'
_publ_section_title
;
 Sulfonium Polyoxometalates: A New Class of Solid-State Photochromic
 Hybrid Organic-Inorganic Materials
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              555
_journal_page_last               557
_journal_paper_doi               10.1021/ic302477p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'Mo8 O26.C8 H32 N4'
_chemical_formula_sum            'C4 H16 Mo4 N2 O13'
_chemical_formula_weight         683.9
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.157(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8352(5)
_cell_length_b                   21.164(2)
_cell_length_c                   10.0444(9)
_cell_measurement_temperature    296
_cell_volume                     1607.7(2)
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type  'Nonius CCD'
_diffrn_measurement_method       'φ , ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.023
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51887
_diffrn_reflns_theta_full        37.49
_diffrn_reflns_theta_max         37.49
_diffrn_reflns_theta_min         5.1
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_T_max  0.6884
_exptl_absorpt_correction_T_min  0.4434
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'Jana2006  (Petricek, Dusek & Palatinus, 2000)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.8248
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.62
_refine_ls_extinction_coef       11800(300)
_refine_ls_extinction_method
'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    1.00
_refine_ls_goodness_of_fit_ref   0.94
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    60
_refine_ls_number_parameters     213
_refine_ls_number_reflns         8395
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.0025
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.001936I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0666
_reflns_number_gt                6264
_reflns_number_total             8395
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic302477p_si_002_1.cif
_cod_data_source_block           II
_cod_database_code               4333644
_cod_database_fobs_code          4333644
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
Mo1 Mo 0.40644(2) 0.397858(7) 0.203784(15) Uani 0.01932(4) 4 1 d
Mo2 Mo 0.242097(19) 0.402336(6) 0.468547(14) Uani 0.01740(4) 4 1 d
Mo3 Mo 0.52548(2) 0.451192(7) 0.770319(14) Uani 0.01843(4) 4 1 d
Mo4 Mo 0.685025(18) 0.448802(6) 0.507124(14) Uani 0.01501(4) 4 1 d
O1 O 0.48089(19) 0.33704(6) 0.12371(13) Uani 0.0292(4) 4 1 d
O2 O 0.66413(17) 0.39489(6) 0.37340(13) Uani 0.0213(4) 4 1 d
O3 O 0.34073(17) 0.35405(6) 0.34788(12) Uani 0.0207(3) 4 1 d
O4 O 0.19970(19) 0.41555(7) 0.10202(15) Uani 0.0283(4) 4 1 d
O5 O 0.53017(17) 0.46998(6) 0.16036(13) Uani 0.0212(3) 4 1 d
O6 O 0.39663(14) 0.47629(5) 0.37596(12) Uani 0.0170(3) 4 1 d
O7 O 0.53619(16) 0.40380(5) 0.60370(12) Uani 0.0173(3) 4 1 d
O8 O 0.19447(18) 0.34483(6) 0.57107(14) Uani 0.0279(4) 4 1 d
O9 O 0.04470(17) 0.42195(7) 0.35991(14) Uani 0.0256(4) 4 1 d
O10 O 0.27213(15) 0.47671(5) 0.59167(12) Uani 0.0177(3) 4 1 d
O11 O 0.3933(2) 0.40271(7) 0.83400(15) Uani 0.0301(4) 4 1 d
O12 O 0.73574(19) 0.43994(7) 0.86939(14) Uani 0.0291(4) 4 1 d
O13 O 0.88619(17) 0.43565(6) 0.61496(13) Uani 0.0235(4) 4 1 d
N1 N 0.2034(3) 0.26105(9) 0.78676(19) Uani 0.0365(6) 4 1 d
C1 C -0.0664(4) 0.30341(14) 0.8311(3) Uani 0.0601(12) 4 1 d
C2 C 0.1143(4) 0.27735(12) 0.8940(3) Uani 0.0450(9) 4 1 d
C3 C 0.3884(3) 0.23766(12) 0.8344(3) Uani 0.0424(8) 4 1 d
C4 C 0.4567(5) 0.22318(18) 0.7115(4) Uani 0.0760(15) 4 1 d
N2 N 0.1091(2) 0.49822(9) 0.85738(17) Uani 0.0323(5) 4 1 d
H1 H -0.135841 0.302405 0.899314 Uiso 0.0722 4 1 d
H2 H -0.056393 0.347107 0.801785 Uiso 0.0722 4 1 d
H3 H -0.12536 0.277773 0.751022 Uiso 0.0722 4 1 d
H4 H 0.184769 0.308743 0.956652 Uiso 0.0541 4 1 d
H5 H 0.10466 0.23954 0.947954 Uiso 0.0541 4 1 d
H6 H 0.199132 0.297319 0.725313 Uiso 0.0438 4 1 d
H7 H 0.131684 0.230326 0.723021 Uiso 0.0438 4 1 d
H8 H 0.391067 0.199206 0.889265 Uiso 0.0509 4 1 d
H9 H 0.462608 0.270174 0.890753 Uiso 0.0509 4 1 d
H10 H 0.578327 0.207513 0.74264 Uiso 0.0911 4 1 d
H11 H 0.381896 0.190884 0.65479 Uiso 0.0911 4 1 d
H12 H 0.454418 0.261663 0.656844 Uiso 0.0911 4 1 d
H13 H 0.0062(9) 0.5237(4) 0.8616(15) Uiso 0.147(18) 4 1 d
H14 H 0.145257 0.47168 0.940836 Uiso 0.0388 4 1 d
H15 H 0.078002 0.470936 0.774862 Uiso 0.0388 4 1 d
H16 H 0.207548 0.526371 0.852199 Uiso 0.0388 4 1 d
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mo -1.6832 0.6857 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
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
O1 Mo1 O2 . . 89.22(5)
O1 Mo1 O3 . . 100.71(6)
O1 Mo1 O4 . . 105.71(7)
O1 Mo1 O5 . . 103.80(7)
O1 Mo1 O6 . . 159.93(5)
O2 Mo1 O3 . . 77.32(5)
O2 Mo1 O4 . . 165.07(6)
O2 Mo1 O5 . . 77.88(5)
O2 Mo1 O6 . . 70.78(4)
O3 Mo1 O4 . . 99.13(7)
O3 Mo1 O5 . . 144.60(5)
O3 Mo1 O6 . . 73.97(5)
O4 Mo1 O5 . . 98.36(6)
O4 Mo1 O6 . . 94.29(6)
O5 Mo1 O6 . . 74.23(5)
O3 Mo2 O6 . . 76.39(5)
O3 Mo2 O7 . . 82.79(5)
O3 Mo2 O8 . . 101.08(6)
O3 Mo2 O9 . . 100.15(6)
O3 Mo2 O10 . . 145.74(5)
O6 Mo2 O7 . . 71.73(4)
O6 Mo2 O8 . . 161.53(5)
O6 Mo2 O9 . . 93.49(6)
O6 Mo2 O10 . . 73.99(5)
O7 Mo2 O8 . . 89.82(5)
O7 Mo2 O9 . . 163.95(6)
O7 Mo2 O10 . . 71.93(4)
O8 Mo2 O9 . . 104.94(7)
O8 Mo2 O10 . . 101.56(6)
O9 Mo2 O10 . . 98.46(6)
O5 Mo3 O6 3_666 3_666 76.96(5)
O5 Mo3 O7 3_666 . 145.26(5)
O5 Mo3 O10 3_666 . 81.38(4)
O5 Mo3 O11 3_666 . 99.88(7)
O5 Mo3 O12 3_666 . 100.84(6)
O6 Mo3 O7 3_666 . 73.84(5)
O6 Mo3 O10 3_666 . 71.04(4)
O6 Mo3 O11 3_666 . 158.18(5)
O6 Mo3 O12 3_666 . 95.07(6)
O7 Mo3 O10 . . 71.67(5)
O7 Mo3 O11 . . 100.25(6)
O7 Mo3 O12 . . 100.10(6)
O10 Mo3 O11 . . 87.15(6)
O10 Mo3 O12 . . 165.21(6)
O11 Mo3 O12 . . 106.70(7)
O2 Mo4 O6 . . 81.26(5)
O2 Mo4 O6 . 3_666 156.66(5)
O2 Mo4 O7 . . 96.67(6)
O2 Mo4 O10 . 3_666 97.60(6)
O2 Mo4 O13 . . 105.76(6)
O6 Mo4 O6 . 3_666 75.41(4)
O6 Mo4 O7 . . 77.83(4)
O6 Mo4 O10 . 3_666 77.49(4)
O6 Mo4 O13 . . 172.95(6)
O6 Mo4 O7 3_666 . 77.76(5)
O6 Mo4 O10 3_666 3_666 78.32(5)
O6 Mo4 O13 3_666 . 97.56(5)
O7 Mo4 O10 . 3_666 149.14(5)
O7 Mo4 O13 . . 100.37(6)
O10 Mo4 O13 3_666 . 101.85(6)
Mo1 O2 Mo4 . . 116.51(6)
Mo1 O3 Mo2 . . 117.42(6)
Mo1 O5 Mo3 . 3_666 115.90(7)
Mo1 O6 Mo2 . . 86.61(4)
Mo1 O6 Mo3 . 3_666 86.45(4)
Mo1 O6 Mo4 . . 91.44(4)
Mo1 O6 Mo4 . 3_666 163.97(5)
Mo2 O6 Mo3 . 3_666 162.74(5)
Mo2 O6 Mo4 . . 97.66(4)
Mo2 O6 Mo4 . 3_666 90.99(5)
Mo3 O6 Mo4 3_666 . 98.30(4)
Mo3 O6 Mo4 3_666 3_666 91.32(4)
Mo4 O6 Mo4 . 3_666 104.59(4)
Mo2 O7 Mo3 . . 104.14(6)
Mo2 O7 Mo4 . . 110.06(5)
Mo3 O7 Mo4 . . 109.73(5)
Mo2 O8 H6 . . 160.7
Mo2 O9 H13 . 3_566 127.28(19)
Mo2 O10 Mo3 . . 103.40(5)
Mo2 O10 Mo4 . 3_666 109.60(6)
Mo3 O10 Mo4 . 3_666 110.54(5)
C2 N1 C3 . . 116.87(18)
N1 C2 C1 . . 110.8(2)
N1 C3 C4 . . 109.3(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mo1 O1 . 1.6997(15)
Mo1 O2 . 2.2769(12)
Mo1 O3 . 1.8998(14)
Mo1 O4 . 1.7155(13)
Mo1 O5 . 1.9187(13)
Mo1 O6 . 2.4128(12)
Mo2 O3 . 1.8975(14)
Mo2 O6 . 2.3172(13)
Mo2 O7 . 2.3489(12)
Mo2 O8 . 1.6976(15)
Mo2 O9 . 1.6948(12)
Mo2 O10 . 1.9775(12)
Mo3 O5 3_666 1.9018(13)
Mo3 O6 3_666 2.3142(13)
Mo3 O7 . 1.9717(13)
Mo3 O10 . 2.3642(11)
Mo3 O11 . 1.6971(17)
Mo3 O12 . 1.7040(14)
Mo4 O2 . 1.7372(13)
Mo4 O6 . 2.3713(11)
Mo4 O6 3_666 2.1668(12)
Mo4 O7 . 1.9493(13)
Mo4 O10 3_666 1.9382(12)
Mo4 O13 . 1.6859(12)
N1 C2 . 1.470(4)
N1 C3 . 1.487(3)
N1 H6 . 0.98
N1 H7 . 0.98
C1 C2 . 1.497(4)
C1 H1 . 0.98
C1 H2 . 0.98
C1 H3 . 0.98
C2 H4 . 0.98
C2 H5 . 0.98
C3 C4 . 1.500(5)
C3 H8 . 0.98
C3 H9 . 0.98
C4 H10 . 0.98
C4 H11 . 0.98
C4 H12 . 0.98
N2 H13 . 0.980(9)
N2 H14 . 0.987
N2 H15 . 0.987
N2 H16 . 0.987
