Phosphate Enriched Polyoxometalate Based Ionic Salts for Proton Conduction
Dey, Chandan; Banerjee, Rahul; Kundu, Tanay; Aiyappa, Harshitha Barike; RSC Adv.  (2014) –; doi:10.1039/C4RA07598F

data_7219003
_publ_section_title
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 Phosphate Enriched Polyoxometalate Based Ionic Salts for Proton
 Conduction
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA07598F
_journal_year                    2014
_chemical_formula_moiety         '5(C2 H10 N2), Mo12 Ni O62 P8, 5.5(O)'
_chemical_formula_sum            'C10 H50 Mo12 N10 Ni O67.5 P8'
_chemical_formula_weight         2848.19
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.20 svn.r3092 for OlexSys, GUI svn.r4949)
;
_audit_update_record
;
2014-11-23 deposited with the CCDC.
2014-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                87.199(12)
_cell_angle_beta                 69.838(11)
_cell_angle_gamma                65.002(11)
_cell_formula_units_Z            1
_cell_length_a                   11.874(8)
_cell_length_b                   13.373(9)
_cell_length_c                   13.817(10)
_cell_measurement_reflns_used    3748
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1855(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9953
_diffrn_measured_fraction_theta_max 0.9089
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21120
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.58
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.501
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.808594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0689 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.8086.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.5503
_exptl_crystal_description       Block
_exptl_crystal_F_000             1353.2581
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         5.9207
_refine_diff_density_min         -1.7470
_refine_diff_density_rms         0.4533
_refine_ls_d_res_high            0.7510
_refine_ls_d_res_low             12.8859
_refine_ls_goodness_of_fit_ref   1.0128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     482
_refine_ls_number_reflns         8341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0128
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+5.5510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5991
_reflns_number_total             8341
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra07598f2.cif
_cod_data_source_block           Ni-POM-EN
_cod_original_cell_volume        1854(2)
_cod_database_code               7219003
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H3c,H3d,H3e} of N3, {H4c,H4d,H4e} of N4
 At 1.5 times of:
  {H2c,H2d,H2e} of N2, {H1c,H1d,H1e} of N1, {H5c,H5d,H5e} of N5
2. Others
 Fixed Sof: O36(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b)
3.b Idealised Me refined as rotating group:
 N1(H1c,H1d,H1e), N2(H2c,H2d,H2e), N3(H3c,H3d,H3e), N4(H4c,H4d,H4e), N5(H5c,
 H5d,H5e)
;
_olex2_submission_special_instructions 'No special instructions were received'