Surface Atom Regulation on Polyoxometalate Electrocatalyst for Simultaneous Low-Voltage H<sub>2</sub> Production and Phenol Degradation.
Zheng, Yang; Xu, Xinxin; ACS applied materials & interfaces  (2020) –; doi:10.1021/acsami.0c14431

data_4518239
_publ_section_title
;
 Surface Atom Regulation on Polyoxometalate Electrocatalyst for
 Simultaneous Low-Voltage H<sub>2</sub> Production and Phenol Degradation.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.0c14431
_journal_year                    2020
_chemical_formula_moiety         'C46 H46 Mo5 N8 Ni2 O27 P2, 5(H2 O), 2(O)'
_chemical_formula_sum            'C46 H56 Mo5 N8 Ni2 O34 P2'
_chemical_formula_weight         1924.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-08-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.360(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6913(3)
_cell_length_b                   21.5989(5)
_cell_length_c                   26.9587(10)
_cell_measurement_reflns_used    14594
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.5370
_cell_measurement_theta_min      3.6010
_cell_volume                     6795.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0359
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -2.00  82.00   1.00    7.50    --   14.24  57.00-150.00   84
  2  \w    -12.00  82.00   1.00    7.50    --   14.24  77.00 150.00   94
  3  \w      7.00  42.00   1.00    7.50    --   14.24  57.00 -90.00   35
  4  \w    -55.00  26.00   1.00    7.50    --   14.24 -38.00  60.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258464000
_diffrn_orient_matrix_UB_12      -0.0292118000
_diffrn_orient_matrix_UB_13      0.0050373000
_diffrn_orient_matrix_UB_21      0.0468131000
_diffrn_orient_matrix_UB_22      0.0148614000
_diffrn_orient_matrix_UB_23      0.0130116000
_diffrn_orient_matrix_UB_31      -0.0288779000
_diffrn_orient_matrix_UB_32      -0.0020674000
_diffrn_orient_matrix_UB_33      0.0223590000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            45334
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.069
_diffrn_reflns_theta_min         3.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       block
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         15877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+8.9611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12841
_reflns_number_total             15877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c14431_si_002.cif
_cod_data_source_block           NiP2Mo5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Green' was changed
to 'green' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               4518239
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ni1 Mo1 P1 N1 C1 O1'
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.676
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O4W(0.5) H4WA(0.5) H4WB(0.5) O6W(0.5) H6WA(0.5) H6WB(0.5) O7W(0.5)
 O10W(0.5) O11W(0.5) O12W(0.5)
3.a Free rotating group:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O8W(H8WA,
 H8WB), O9W(H9WA,H9WB)
3.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.c Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C4AA(H4AA,H4AB), C5AA(H5AA,H5AB)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22A), C23(H23), C24(H24A), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C82(H82)
3.e Tetrahedral OH refined with riding coordinates:
 O22(H22)
3.f Idealised tetrahedral OH refined as rotating group:
 O24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.072
_oxdiff_exptl_absorpt_empirical_full_min 0.918