Molybdophosphate derived MoP based electrocatalyst as cathode for Sn‒H+ battery to generate H2 and electricity simultaneously
Wang, Lusha; Dong, Baichuan; Xu, Xinxin; Wang, Yi; Journal of Solid State Chemistry 277 (2019) 602–610; doi:10.1016/j.jssc.2019.07.017

data_1561682
_publ_section_title
;
 Molybdophosphate derived MoP based electrocatalyst as cathode for Sn--H+
 battery to generate H2 and electricity simultaneously
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              602
_journal_page_last               610
_journal_paper_doi               10.1016/j.jssc.2019.07.017
_journal_volume                  277
_journal_year                    2019
_chemical_formula_moiety
'C144 H112 Mo12 N12 O86 P12 Zn11, 7(H2 O), 2(O0.75)'
_chemical_formula_sum            'C144 H126 Mo12 N12 O94.5 P12 Zn11'
_chemical_formula_weight         5778.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                75.265(2)
_cell_angle_beta                 82.738(2)
_cell_angle_gamma                62.625(2)
_cell_formula_units_Z            1
_cell_length_a                   15.5443(10)
_cell_length_b                   16.3850(10)
_cell_length_c                   21.9653(14)
_cell_measurement_reflns_used    9558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.971
_cell_volume                     4804.3(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76476
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.940
_exptl_absorpt_coefficient_mu    2.298
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1043 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.7524. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1313
_refine_ls_number_reflns         22036
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+7.0014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                17889
_reflns_number_total             22036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yjssc_20856_ZnP4Mo6_mmc2.cif
_cod_data_source_block           15a
_cod_original_formula_sum        'C144 H126 Mo12 N12 O94.50 P12 Zn11'
_cod_database_code               1561682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C37A \\sim C38A
\\sim C39A \\sim C40A \\sim C41A \\sim C42A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C13) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C15) = Uanis(C14) =
Uanis(C13A) = Uanis(C18A) = Uanis(C17A) = Uanis(C16A) = Uanis(C15A) =
Uanis(C14A)
3. Others
 Fixed Sof: C13(0.5) C18(0.5) H18(0.5) C17(0.5) H17(0.5) C16(0.5) H16(0.5)
 C15(0.5) H15(0.5) C14(0.5) H14(0.5) C37(0.5) C38(0.5) H38(0.5) C39(0.5)
 H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) O3W(0.5)
 H3WA(0.5) H3WB(0.5) C37A(0.5) C38A(0.5) H38A(0.5) C39A(0.5) H39A(0.5)
 C40A(0.5) H40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5) H42A(0.5) C13A(0.5)
 C18A(0.5) H18A(0.5) C17A(0.5) H17A(0.5) C16A(0.5) H16A(0.5) C15A(0.5)
 H15A(0.5) C14A(0.5) H14A(0.5) O5W(0.5) O6W(0.25)
4.a Free rotating group:
 O0AA(H0AA,H0AB), O4W(H4WA,H4WB), O3W(H3WA,H3WB), O1W(H1WA,H1WB)
4.b Rotating group:
 O3(H3A,H3B), O4(H4A,H4B), O6(H6A,H6B), O12(H12A,H12B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C9(H9), C10(H10), C18(H18), C17(H17),
 C16(H16), C15(H15), C14(H14), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C29(H29), C30(H30), C33(H33), C34(H34), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C53(H53), C54(H54), C57(H57), C58(H58),
 C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70),
  C71(H71), C72(H72), C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A),
 C42A(H42A), C18A(H18A), C17A(H17A), C16A(H16A), C15A(H15A), C14A(H14A)
4.d Fitted hexagon refined as free rotating group:
 C13(C18,C17,C16,C15,C14), C37(C38,C39,C40,C41,C42), C37A(C38A,C39A,C40A,C41A,
 C42A), C13A(C18A,C17A,C16A,C15A,C14A)
;
_shelx_res_checksum              70519
_shelx_hkl_checksum              95742
_olex2_submission_special_instructions 'No special instructions were received'