[Ni(OH)3W6O18(OCH2)3CCH2OH]4-: the first tris-functionalized Anderson-type heteropolytungstate
Nadiia I. Gumerova; Alexander Roller; Annette Rompel; Chemical Communications 52 (2016) 9263–9266; doi:10.1039/c6cc04326g

data_7121015
_publ_section_title
;
 [Ni(OH)3W6O18(OCH2)3CCH2OH]4-: the first tris-functionalized
 Anderson-type heteropolytungstate
;
_journal_name_full               'Chemical Communications'
_journal_page_first              9263
_journal_page_last               9266
_journal_paper_doi               10.1039/c6cc04326g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C5 H24 Na2 Ni O31 W6, 2(C4 H12 N), 3(H2 O)'
_chemical_formula_sum            'C13 H54 N2 Na2 Ni O34 W6'
_chemical_formula_weight         1990.37
_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   mixed
_atom_sites_solution_primary     heavy
_cell_angle_alpha                113.7330(12)
_cell_angle_beta                 102.5434(12)
_cell_angle_gamma                90.4790(12)
_cell_formula_units_Z            1
_cell_length_a                   9.6825(4)
_cell_length_b                   10.3943(5)
_cell_length_c                   11.7580(6)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.189
_cell_measurement_theta_min      2.937
_cell_volume                     1051.34(9)
_computing_cell_refinement       'APEX2 v2013.6-2'
_computing_data_collection       'APEX2 v2013.6-2'
_computing_data_reduction        'APEX2 v2013.6-2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            46417
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'INCOATEC microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.905
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0669 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.7613.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.144
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.829
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3820
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.319
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0163P)^2^+4.6476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3816
_reflns_number_total             3820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Chem-Commun-2016-52-9263.cif
_cod_data_source_block           mo_emasni37_4_p-1
_cod_database_code               7121015
_shelx_estimated_absorpt_t_max   0.294
_shelx_estimated_absorpt_t_min   0.175
_shelx_res_checksum              83050