Synthesis and characterization of the `Japanese rice-ball'-shaped Molybdenum Blue Na~4~[Mo~2~O~2~(OH)~4~(C~6~H~4~NO~2~)~2~]~2~[Mo~120~Ce~6~O~366~H~12~(OH)~2~(H~2~O)~76~]∼ 200H~2~O
Al-Sayed, Emir; Tanuhadi, Elias; Giester, Gerald; Rompel, Annette; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S2053229622003369

data_2022596
_publ_section_title
;
 Synthesis and characterization of the `Japanese rice-ball'-shaped
 Molybdenum Blue
 Na~4~[Mo~2~O~2~(OH)~4~(C~6~H~4~NO~2~)~2~]~2~[Mo~120~Ce~6~O~366~H~12~(OH)~2~(H~2~O)~76~]\\sim
 200H~2~O
;
_journal_coeditor_code           KY3215
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622003369
_journal_volume                  78
_journal_year                    2022
_chemical_formula_moiety
'Ce6 Mo120 O444, 2(C12 H8 Mo2 N2 Na2 O10.5), 36(O)'
_chemical_formula_sum            'C24 H588 Ce6 Mo124 N4 Na4 O664'
_chemical_formula_weight         24391.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.145(4)
_cell_angle_gamma                90
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_cell_length_b                   38.896(7)
_cell_length_c                   31.734(6)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      20.538
_cell_measurement_theta_min      2.192
_cell_volume                     62048(2)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009),
<i>DIAMOND</i> (Brandenburg, 2006) and
<i>shelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            373860
_diffrn_reflns_theta_full        20.885
_diffrn_reflns_theta_max         20.885
_diffrn_reflns_theta_min         1.063
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.974
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_description       block
_exptl_crystal_F_000             46688
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         3.028
_refine_diff_density_min         -2.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2814
_refine_ls_number_reflns         32484
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+9956.6523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2335
_reflns_number_gt                23243
_reflns_number_total             32484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3215sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        62047(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2022596
_shelx_hkl_checksum              49831
_shelx_res_checksum              75680
_shelx_fab_checksum              86479
_cod_database_fobs_code 2022596