Iron(II) and copper(II) paratungstates B: a single-crystal X-ray diffraction study
Gumerova, Nadiia I.; Dobrov, Anatolie; Roller, Alexander; Rompel, Annette; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618010021

data_2021254
_publ_section_title
;
 Iron(II) and copper(II) paratungstates B: a single-crystal X-ray
 diffraction study
;
_journal_coeditor_code           JR3015
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618010021
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'Na5 Fe2.5 [W12 O40 (O H)2], 36H2 O'
_chemical_formula_moiety         'Fe2.5 H54 Na5 O71 W12, 7(H2 O)'
_chemical_formula_sum            'Fe2.5 H62 Na5 O78 W12'
_chemical_formula_weight         3771.27
_chemical_name_common            'sodium-iron(II) pararungstateB'
_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   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                92.9341(14)
_cell_angle_beta                 100.6938(14)
_cell_angle_gamma                94.1698(15)
_cell_formula_units_Z            2
_cell_length_a                   12.3758(6)
_cell_length_b                   14.7752(7)
_cell_length_c                   18.8919(8)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      2.18
_cell_volume                     3378.1(3)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection       APEX3
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38068
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'sealed xray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.022
_exptl_absorpt_correction_T_max  0.0439
_exptl_absorpt_correction_T_min  0.0117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_density_diffrn    3.708
_exptl_crystal_description       needle
_exptl_crystal_F_000             3388
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.567
_refine_diff_density_min         -1.254
_refine_ls_extinction_coef       0.000312(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2016)
;
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         12318
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+7.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                10876
_reflns_number_total             12318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3015sup1.cif
_cod_data_source_block           mo_ando241_p-1
_cod_original_formula_sum        'Fe2.50 H62 Na5 O78 W12'
_cod_database_code               2021254
_shelx_estimated_absorpt_t_min   0.048
_shelx_estimated_absorpt_t_max   0.472
_cod_database_fobs_code 2021254