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_7219004
_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         'H8 Mo12 Ni O62 P8, C10 H10 N2, 5(O)'
_chemical_formula_sum            'C10 H18 Mo12 N2 Ni O67 P8'
_chemical_formula_weight         2695.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                90
_cell_angle_beta                 92.441(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.559(6)
_cell_length_b                   23.664(9)
_cell_length_c                   23.421(9)
_cell_measurement_reflns_used    8816
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     8062(5)
_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 0.9958
_diffrn_measured_fraction_theta_max 0.9309
_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  0.1095
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            90583
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.585066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0870 before and 0.0379 after correction.
The Ratio of minimum to maximum transmission is 0.5851.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.2211
_exptl_crystal_description       block
_exptl_crystal_F_000             5044.9916
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         4.7298
_refine_diff_density_min         -1.4900
_refine_diff_density_rms         0.3472
_refine_ls_d_res_high            0.7476
_refine_ls_d_res_low             11.8322
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0820
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     884
_refine_ls_number_reflns         18817
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0819
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.1535
_refine_ls_shift/su_mean         0.0028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+52.7970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2004
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                15078
_reflns_number_total             18817
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra07598f2.cif
_cod_data_source_block           Ni-POM-BP
_cod_database_code               7219004
_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 O(H) groups
2. Restrained distances
 O29-H29
 0.85 with sigma of 0.01
 P8-H29
 1.966695 with sigma of 0.02
 Mo12-H29
 2.553208 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), N1(H1a),
 N2(H2a)
3.b Idealised tetrahedral OH refined as rotating group:
 O15(H15), O24(H24), O27(H27), O50(H50), O52(H52), O55(H55), O58(H58)
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_olex2_submission_special_instructions 'No special instructions were received'