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_1543965
_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, H3 O, C20 H32 N2, C10 H12 N'
_chemical_formula_sum            'C30 H53 Mo8 N3 O28'
_chemical_formula_weight         1671.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.868(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6049(10)
_cell_length_b                   21.9318(13)
_cell_length_c                   18.1934(10)
_cell_measurement_reflns_used    7852
_cell_measurement_temperature    291.15
_cell_measurement_theta_max      26.3153
_cell_measurement_theta_min      2.9351
_cell_volume                     4939.3(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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  -87.00  -43.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2218  145.0000   89.0000 44

  2 omega    0.00   55.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8000   77.0000   30.0000 55

  3 omega   -4.00   88.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8000   37.0000  150.0000 92

  4 omega  -49.00    3.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8000  -77.0000 -150.0000 52
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0425176000
_diffrn_orient_matrix_UB_12      0.0143888000
_diffrn_orient_matrix_UB_13      -0.0139048000
_diffrn_orient_matrix_UB_21      0.0181012000
_diffrn_orient_matrix_UB_22      -0.0288680000
_diffrn_orient_matrix_UB_23      -0.0102845000
_diffrn_orient_matrix_UB_31      -0.0336648000
_diffrn_orient_matrix_UB_32      0.0026978000
_diffrn_orient_matrix_UB_33      -0.0357910000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22253
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_density_diffrn    2.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.2322
_exptl_crystal_size_mid          0.1737
_exptl_crystal_size_min          0.1304
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         10083
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+6.0378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                7271
_reflns_number_total             10083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2014-409B-418-426-10.cif
_cod_data_source_block           10
_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               1543965