Templated fabrication, isomer recognition of series of 1,1'-(alkane-1,omega-diyl)-bis(3-methylimidazolium)-induced polyoxometalates (omega = 1-11)
Hai-Juan Du; Li-Wei Mi; Zhong-Cheng Yue; Yun-Yin Niu; Hong-Wei Hou; Inorganica Chimica Acta  (2014) 418–426; doi:10.1016/j.ica.2013.09.050

data_1543973
_publ_section_title
;
 Templated fabrication, isomer recognition of series of
 1,1'-(alkane-1,omega-diyl)-bis(3-methylimidazolium)-induced
 polyoxometalates (omega = 1-11)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              418
_journal_page_last               426
_journal_paper_doi               10.1016/j.ica.2013.09.050
_journal_volume                  409B
_journal_year                    2014
_chemical_formula_moiety         'Mo8 O26, H2 O, 2(C16 H28 N4)'
_chemical_formula_sum            'C24 H46 Mo8 N6 O27'
_chemical_formula_weight         1618.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.584(4)
_cell_angle_beta                 84.439(4)
_cell_angle_gamma                71.601(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1983(5)
_cell_length_b                   11.6038(6)
_cell_length_c                   20.4333(9)
_cell_measurement_reflns_used    6830
_cell_measurement_temperature    291.15
_cell_measurement_theta_max      26.3105
_cell_measurement_theta_min      3.0018
_cell_volume                     2275.2(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -42.00   -9.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  101.0000  132.0000 66

  2 omega   16.00   62.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885 -101.0000 -132.0000 92

  3 omega    4.00   49.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -77.0000  -30.0000 90

  4 omega   36.00   91.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   37.0000  -60.0000 110

  5 omega  -47.00   93.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885    0.0000  -90.0000 280

  6 omega   -7.00   68.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   77.0000   90.0000 150
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0567639000
_diffrn_orient_matrix_UB_12      -0.0198002000
_diffrn_orient_matrix_UB_13      -0.0055284000
_diffrn_orient_matrix_UB_21      0.0004426000
_diffrn_orient_matrix_UB_22      -0.0271342000
_diffrn_orient_matrix_UB_23      0.0328861000
_diffrn_orient_matrix_UB_31      -0.0466175000
_diffrn_orient_matrix_UB_32      0.0552487000
_diffrn_orient_matrix_UB_33      0.0106489000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17052
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9286
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.0288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                6543
_reflns_number_total             9286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2014-409B-418-426-8.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_journal_paper_doi' value
'http://dx.doi.org/10.1016/j.ica.2013.09.050' was changed to
'10.1016/j.ica.2013.09.050'.

Automatic conversion script
Id: cif_fix_values 6433 2018-09-21 13:16:33Z andrius 
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_cod_database_code               1543973