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_1543968
_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         '2(Mo4 O13), 2(C11 H18 N4)'
_chemical_formula_sum            'C22 H36 Mo8 N8 O26'
_chemical_formula_weight         1596.11
_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                96.707(5)
_cell_angle_beta                 96.709(5)
_cell_angle_gamma                116.082(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3059(8)
_cell_length_b                   10.9132(9)
_cell_length_c                   21.2906(10)
_cell_measurement_reflns_used    8870
_cell_measurement_temperature    291.15
_cell_measurement_theta_max      26.3149
_cell_measurement_theta_min      2.9769
_cell_volume                     2097.7(3)
_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 16.2542
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -44.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642  -77.0000  150.0000 90

  2 omega   -8.00   88.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642   77.0000  -90.0000 96

  3 omega  -54.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642  -37.0000    0.0000 40

  4 omega  -47.00   36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642  -37.0000   30.0000 83

  5 omega   22.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2642 -132.0000   72.0000 57

  6 omega  -81.00  -56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8892  -37.0000  -60.0000 25

  7 omega  -82.00  -55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8892  136.0000  104.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0773926000
_diffrn_orient_matrix_UB_12      0.0379373000
_diffrn_orient_matrix_UB_13      0.0102622000
_diffrn_orient_matrix_UB_21      0.0089870000
_diffrn_orient_matrix_UB_22      -0.0030916000
_diffrn_orient_matrix_UB_23      -0.0325784000
_diffrn_orient_matrix_UB_31      -0.0042169000
_diffrn_orient_matrix_UB_32      0.0630925000
_diffrn_orient_matrix_UB_33      -0.0002470000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16409
_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    2.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97660
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.014
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         8552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0734P)^2^+14.8413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                7089
_reflns_number_total             8552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2014-409B-418-426-3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 4624 2016-04-14 12:54:50Z antanas 

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 
;
_cod_database_code               1543968