Crystal structure of a new polyoxometalate (POM) compound with a high level of crystallographic disorder
Skorepova, Eliska; Harchani, Ali; Ftini, Mohamed Mongi; Dušek, Michal; Haddad, Amor; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229619015596

data_2021964
_publ_section_title
;
 Crystal structure of a new polyoxometalate (POM) compound with a high
 level of crystallographic disorder
;
_journal_coeditor_code           YD3001
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619015596
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C7 H10 N O)8.5 [P2 Mo5 O23]2, 3H2 O'
_chemical_formula_sum            'C59.5 H76.5 Mo10 N8.5 O60.029 P4'
_chemical_formula_weight         2993.5
_chemical_name_systematic
;
Nonakis(2-methoxyaniline) bis(diphosphopentamolybdate) trihydrate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                89.1396(7)
_cell_angle_beta                 78.1097(7)
_cell_angle_gamma                75.4959(8)
_cell_formula_units_Z            2
_cell_length_a                   14.8316(2)
_cell_length_b                   15.26790(10)
_cell_length_c                   23.2370(2)
_cell_measurement_reflns_used    14565
_cell_measurement_temperature    95.0(6)
_cell_measurement_theta_max      73.58
_cell_measurement_theta_min      4.01
_cell_volume                     4981.24(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND3 (Brandenburg & Putz, 2005), Mercury (Macrae <i>et al.</i>,
2008)
and Discovery Studio Visualizer (https://www.3dsbiovia.com/)
;
_computing_structure_refinement
;
JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2014)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      95
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2027
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku OD SuperNova Dual source diffractometer with an AtlasS2 detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35243
_diffrn_reflns_theta_full        73.08
_diffrn_reflns_theta_max         74.16
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    11.567
_exptl_absorpt_correction_T_max  0.641
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.9958
_exptl_crystal_description       'polygonal shape'
_exptl_crystal_F_000             2950
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.064
_refine_diff_density_max         7.49
_refine_diff_density_min         -4.98
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    2.93
_refine_ls_goodness_of_fit_ref   2.74
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    252
_refine_ls_number_parameters     557
_refine_ls_number_reflns         19576
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.2124
_refine_ls_wR_factor_ref         0.2187
_reflns_number_gt                16182
_reflns_number_total             19576
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            yd3001sup1.cif
_cod_data_source_block           I
_cod_database_code               2021964
_cod_database_fobs_code 2021964