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_7219005
_publ_section_title
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 Phosphate Enriched Polyoxometalate Based Ionic Salts for Proton
 Conduction
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_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA07598F
_journal_year                    2014
_chemical_formula_moiety         'H2 Mo12 Ni O62 P8, 2(C12 H13 N2),8(O)'
_chemical_formula_sum            'C24 H28 Mo12 N4 Ni O70 P8'
_chemical_formula_weight         2950.23
_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'
_audit_creation_date             2014-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.21 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                111.029(12)
_cell_angle_beta                 109.293(12)
_cell_angle_gamma                101.693(13)
_cell_formula_units_Z            1
_cell_length_a                   12.891(10)
_cell_length_b                   13.743(10)
_cell_length_c                   14.234(11)
_cell_measurement_reflns_used    4417
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2069(3)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9827
_diffrn_measured_fraction_theta_max 0.8853
_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  0.0697
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17676
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.70
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.839300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0632 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.8393.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.3681
_exptl_crystal_description       block
_exptl_crystal_F_000             1393.3160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         4.8730
_refine_diff_density_min         -1.5829
_refine_diff_density_rms         0.2763
_refine_ls_d_res_high            0.7517
_refine_ls_d_res_low             11.9445
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0091
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.0068
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -18
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6922
_reflns_number_total             9034
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra07598f2.cif
_cod_data_source_block           Ni-POM-DP
_cod_database_code               7219005
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), N1(H1)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C10(H10a,H10b,H10c)
2.c Idealised tetrahedral OH refined as rotating group:
 O25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'