Copper-containing hybrid compounds based on extremely rare [V2Mo6O26]6– POM as water oxidation catalysts
Buvailo, Halyna I.; Makhankova, Valeriya G.; Kokozay, Vladimir N.; Omelchenko, Irina V.; Shishkina, Svitlana V.; Jezierska, Julia; Pavliuk, Mariia V.; Shylin, Sergii I.; Inorganic Chemistry Frontiers 6 (2019) 1813–; doi:10.1039/C9QI00040B

data_4349996
_publ_section_title
;
 Copper-containing hybrid compounds based on extremely rare [V2Mo6O26]6--
 POM as water oxidation catalysts
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1813
_journal_paper_doi               10.1039/C9QI00040B
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C8 H30 Cu2 Mo6 N6 O28 V2, 2(H4 N), 8(H2 O)'
_chemical_formula_sum            'C8 H54 Cu2 Mo6 N8 O36 V2'
_chemical_formula_weight         1643.19
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-29 deposited with the CCDC.	2019-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.328(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2569(3)
_cell_length_b                   9.1947(2)
_cell_length_c                   21.9132(5)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.4350
_cell_measurement_theta_min      3.5860
_cell_volume                     2238.11(9)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
  1 omega  -86.00  -38.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.2300 -178.0000 -180.0000 48

  2 omega   27.00   69.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   57.0000  150.0000 42

  3 omega   -3.00   44.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   77.0000 -150.0000 47

  4 omega   10.00   44.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   59.0000  -79.0000 34

  5 omega  -42.00   57.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363  -77.0000   60.0000 99

  6 omega    5.00   95.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6363   57.0000   30.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0105267000
_diffrn_orient_matrix_UB_12      0.0459844000
_diffrn_orient_matrix_UB_13      0.0262718000
_diffrn_orient_matrix_UB_21      0.0525512000
_diffrn_orient_matrix_UB_22      0.0276253000
_diffrn_orient_matrix_UB_23      -0.0099743000
_diffrn_orient_matrix_UB_31      -0.0348151000
_diffrn_orient_matrix_UB_32      0.0553952000
_diffrn_orient_matrix_UB_33      -0.0168946000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19449
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         32.268
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.971
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+3.3013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5746
_reflns_number_total             7174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00040b2.cif
_cod_data_source_block           koko786red
_cod_database_code               4349996
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1S-H1SC = N1S-H1SD
 0.85 with sigma of 0.01
 N1S-H1SF = N1S-H1SE
 0.85 with sigma of 0.01
 H1SF-H1SE \\sim H1SF-H1SC \\sim H1SE-H1SC \\sim H1SE-H1SD \\sim H1SF-H1SD
 with sigma of 0.01
 H1SC-H1SD \\sim H1SD-H1SF
 with sigma of 0.01
 H1SD-H1SC \\sim H1SC-H1SE
 with sigma of 0.01
3.a Riding coordinates:
 O1S(H1SA,H1SB), N1S(H1SC,H1SD,H1SE,H1SF), O4S(H4SA,H4SB), O2S(H2SA,H2SB),
 O3S(H3SA,H3SB), O5S(H5SA,H5SB)
3.b Ternary CH refined with riding coordinates:
 N2(H2)
3.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), C1(H1C,H1D), C3(H3C,H3D), C4(H4A,H4B)
;
_olex2_submission_special_instructions 'No special instructions were received'