Structures, electronic properties, reactivity and dynamic studies of three new polyoxometalate compounds.
Harchani, Ali; Kučeráková, Monika; Dušek, Michal; Haddad, Amor; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10965–10975; doi:10.1039/c8dt02205d

data_7046985
_publ_section_title
;
 Structures, electronic properties, reactivity and dynamic studies of
 three new polyoxometalate compounds.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10965
_journal_page_last               10975
_journal_paper_doi               10.1039/c8dt02205d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C6 H24 Mo12 N3 O40.343 P1'
_chemical_formula_sum            'C6 H24 Mo12 N3 O40.343 P'
_chemical_formula_weight         1966
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_audit_update_record
;
2018-06-29 deposited with the CCDC.
2018-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   16.3798(3)
_cell_length_b                   16.3798(3)
_cell_length_c                   50.2781(5)
_cell_measurement_reflns_used    46639
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      3.86
_cell_volume                     11682.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Diamond (Brandenburg & Putz, 2005)'
_computing_publication_material
'Jana2006 (Pet\<r\'i\<cek, Du\<sek & Palatinus, 2014)'
_computing_structure_refinement
'Jana2006 (Pet\<r\'i\<cek, Du\<sek & Palatinus, 2014)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3567
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            57833
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program CrysAlisPro
(Agilent Technologies, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        29.58
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         3.3
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.892
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33b (Rigaku Oxford Diffraction, 2017)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.3534
_exptl_crystal_description       'polygon shape'
_exptl_crystal_F_000             11073
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.51
_refine_ls_extinction_coef       2240(110)
_refine_ls_extinction_method
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    1.70
_refine_ls_goodness_of_fit_ref   1.64
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    32
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0163
_refine_ls_shift/su_max          0.0039
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0004I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0496
_reflns_number_gt                3218
_reflns_number_total             3593
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c8dt02205d2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7046984--7046986.cif.
;
_cod_original_sg_symbol_Hall     '-R 3;-2"c'
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C6 H24 Mo12 N3 O40.343 P1'
_cod_database_code               7046985