Synthesis and properties of charge-transfer solids with cluster units [Mo6X14]2− (X = Br, I)
Saito, Gunzi; Hosoda, Hidemasa; Yoshida, Yukihiro; Hagiwara, Jun; Nishimura, Kazukuni; Yamochi, Hideki; Otsuka, Akihiro; Hiramatsu, Takaaki; Shimazaki, Yuichi; Kirakci, Kaplan; Cordier, Stéphane; Perrin, Christiane; Journal of Materials Chemistry 22 (2012) 19774–; doi:10.1039/c2jm33086e

data_7208624
_publ_section_title
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 Synthesis and properties of charge-transfer solids with cluster units
 [Mo6X14]2&#x2212; (X = Br, I)
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_journal_issue                   37
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              19774
_journal_paper_doi               10.1039/c2jm33086e
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         '2(C10 H8 O4 S4), Br14 Mo6, 4(C7 H5 N1)'
_chemical_formula_sum            'C48 H36 Br14 Mo6 N4 O8 S8'
_chemical_formula_weight         2747.60
_chemical_name_common            (BO)2Mo6Br14(PhCN)3
_chemical_name_systematic
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Molybdate(2-), dodeca-m-bromodibromohexa-, octahedro , salt with
2-(5,6-dihydro-1,3-dithiolo[4,5-b][1,4]dioxin-2-ylidene)-5,6-dihydro-
1,3-dithiolo[4,5-b][1,4]dioxin, compd. with benzonitrile (1:2:4)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.414(4)
_cell_length_b                   21.711(7)
_cell_length_c                   15.958(5)
_cell_measurement_reflns_used    3130
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     3601(2)
_computing_cell_refinement       'MXC(MAC Science)'
_computing_data_collection       'MXC(MAC Science)'
_computing_data_reduction        Crystan
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.372
_diffrn_measured_fraction_theta_max 0.372
_diffrn_measurement_device_type  'MAC SCIENCE MXC^\x^'
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.1997
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9207
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    9.062
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         3157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                3157
_reflns_number_total             3157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2jm33086e.txt
_cod_data_source_block           bo-1
_cod_depositor_comments
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The following automatic conversions were performed:

'_cell_measurement_temperature' value 'Room Temperature' was changed
to '295(2)' - the room/ambient temperature average [293;298] in
Kelvins(K) was taken.

'_diffrn_ambient_temperature' value 'Room
Temperature' was changed to '295(2)' - the room/ambient temperature
average [293;298] in Kelvins(K) was taken.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_sg_symbol_H-M      'P 2(1)/n '
_cod_database_code               7208624