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_2021253
_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          'Na4 Cu3 [W12 O40 (O H)2], 28H2 O'
_chemical_formula_moiety         'Cu3 H36 Na4 O64 W12, 4(H2 O)'
_chemical_formula_sum            'Cu3 H44 Na4 O68 W12'
_chemical_formula_weight         3621.13
_chemical_name_common            'sodium-copper(II) paratungstateB'
_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                113.7710(10)
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_cell_angle_gamma                112.5020(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6516(5)
_cell_length_b                   12.7532(6)
_cell_length_c                   13.0730(5)
_cell_measurement_reflns_used    6027
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      3.04
_cell_volume                     1473.65(11)
_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) and
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
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OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and
shelXle (H\"ubschle <i>et al.</i>,  2011)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0475
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11292
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.109
_diffrn_source                   'sealed xray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.527
_exptl_absorpt_correction_T_max  0.0232
_exptl_absorpt_correction_T_min  0.0037
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;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.080
_exptl_crystal_description       plate
_exptl_crystal_F_000             1607
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.153
_refine_diff_density_min         -1.633
_refine_ls_extinction_coef       0.00022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         5321
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+6.2838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                4720
_reflns_number_total             5321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3015sup1.cif
_cod_data_source_block           ando209_p-1
_cod_database_code               2021253
_shelx_estimated_absorpt_t_min   0.143
_shelx_estimated_absorpt_t_max   0.640
_cod_database_fobs_code 2021253