Synthesis, crystal structure and catalytic activity of Guanidinium cation directed Nickel (II)-containing open Wells‒Dawson 19-tungstodiarsenate (III) [{Ni(H2O)4}2{Na(H2O)}As2W19O67(H2O)]9-
Saini, Mukesh; Gupta, Rakesh; Singh, Surendra; Hussain, Firasat; RSC Adv.  (2015) –; doi:10.1039/C5RA01426C

data_7219731
_publ_section_title
;
 Synthesis, crystal structure and catalytic activity of Guanidinium cation
 directed Nickel (II)-containing open Wells--Dawson 19-tungstodiarsenate
 (III) [{Ni(H2O)4}2{Na(H2O)}As2W19O67(H2O)]9-
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA01426C
_journal_year                    2015
_chemical_formula_sum            'C5 As2 N15 Na2 Ni2 O91 W19'
_chemical_formula_weight         5532.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-12 deposited with the CCDC.
2015-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                84.426(2)
_cell_angle_beta                 84.995(2)
_cell_angle_gamma                66.972(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1357(4)
_cell_length_b                   16.6865(5)
_cell_length_c                   26.3032(6)
_cell_measurement_reflns_used    33876
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.7668
_cell_measurement_theta_min      2.8161
_cell_volume                     5273.2(3)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2011)'
_computing_data_collection       'CrysAlis RED (Oxford, 2011)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2011)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            211119
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    21.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4826
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.142
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         20751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+194.3218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                17902
_reflns_number_total             20751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra01426c2.cif
_cod_data_source_block           shelxl
_cod_database_code               7219731