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_1543972
_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(C15 H26 N4), 2(C7.5 H6 N2), 4(Mo4 O13), 4(O0.5)
;
_chemical_formula_sum            'C45 H90 Mo16 N12 O54'
_chemical_formula_weight         3198.33
_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                92.188(12)
_cell_angle_beta                 98.683(8)
_cell_angle_gamma                112.18(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1362(13)
_cell_length_b                   12.646(4)
_cell_length_c                   19.1345(12)
_cell_measurement_reflns_used    8324
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.1133
_cell_measurement_theta_min      2.9235
_cell_volume                     2233.0(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.0
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.837
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details
;
1 omega  -73.00  -25.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-      -17.1323  124.0000 -140.0000 48

2 omega  -67.00   -1.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-      -17.1323  -77.0000    0.0000 66

3 omega  -73.00  -24.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-      -17.1323  124.0000   39.0000 49

4 omega    4.00   36.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-       19.6323   77.0000 -180.0000 32

5 omega  -49.00   17.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-       19.6323  -37.0000 -180.0000 66

6 omega  -50.00   92.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-       19.6323    0.0000 -150.0000 142

7 omega   -6.00   30.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
-       19.6323   37.0000  -60.0000 36
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185705
_diffrn_orient_matrix_UB_12      0.0080186
_diffrn_orient_matrix_UB_13      0.0376654
_diffrn_orient_matrix_UB_21      0.0297703
_diffrn_orient_matrix_UB_22      0.0604722
_diffrn_orient_matrix_UB_23      -0.000993
_diffrn_orient_matrix_UB_31      -0.0685115
_diffrn_orient_matrix_UB_32      0.0018302
_diffrn_orient_matrix_UB_33      0.0021411
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19732
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.85733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         10078
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0316P)^2^+0.4741P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                8053
_reflns_number_total             10078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2014-409B-418-426-7.cif
_cod_data_source_block           7
_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_original_cell_volume        2232.9(8)
_cod_database_code               1543972