Crystal structure of octakis(<i>N</i>,<i>N</i>-dimethylformamide-κ<i>O</i>)europium(III) tetracosa-μ~2~-oxido-dodecaoxido-μ~12~-phosphato-dodecamolybdate(VI)
Ghandour, Yassine; Hammami, Imen; Najmudin, Shabir; Bonifácio, Cecilia; Belkhiria, Mohamed Salah; Acta Crystallographica Section E 72 (2016) 448–451; doi:10.1107/S2056989016003546

data_2241590
_publ_section_title
;
 Crystal structure of
 octakis(<i>N</i>,<i>N</i>-dimethylformamide-\k<i>O</i>)europium(III)
 tetracosa-\m~2~-oxido-dodecaoxido-\m~12~-phosphato-dodecamolybdate(VI)
;
_journal_coeditor_code           WM5274
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              448
_journal_page_last               451
_journal_paper_doi               10.1107/S2056989016003546
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Eu (C3 H7 N O)8] [P Mo12 O40]'
_chemical_formula_moiety         'C24 H56 Eu1 N8 O8 3+, Mo12 O40 P1 3-'
_chemical_formula_sum            'C24 H56 Eu Mo12 N8 O48 P'
_chemical_formula_weight         2558.97
_chemical_name_systematic
;
Octakis(<i>N</i>,<i>N</i>-dimethylformamide-\k<i>O</i>)europium(III)
tetracosa-\m~2~-oxido-dodecaoxido-\m~12~-phosphato-dodecamolybdate(VI)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9108(10)
_cell_length_b                   18.3506(6)
_cell_length_c                   13.4494(4)
_cell_measurement_reflns_used    9528
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.28
_cell_measurement_theta_min      2.946
_cell_volume                     6641.7(4)
_computing_cell_refinement
;
SAINT (Bruker, 2006)
;
_computing_data_collection
;
APEX2 (Bruker, 2006)
;
_computing_data_reduction
;
SAINT (Bruker, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Putz & Brandenburg,
2014)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88354
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.122
_diffrn_reflns_theta_min         2.220
_exptl_absorpt_coefficient_mu    3.242
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2006)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4888
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.796
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 6924 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
;
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         33285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                19583
_reflns_number_total             33285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5274sup1.cif
_cod_data_source_block           I
_cod_database_code               2241590
_cod_database_fobs_code          2241590
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.609
_shelx_hkl_checksum              94105
_shelx_res_checksum              6981