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_4349997
_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), 5(H2 O)'
_chemical_formula_sum            'C8 H48 Cu2 Mo6 N8 O33 V2'
_chemical_formula_weight         1589.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8618(8)
_cell_length_b                   23.2484(12)
_cell_length_c                   15.7977(8)
_cell_measurement_reflns_used    1102
_cell_measurement_temperature    298
_cell_measurement_theta_max      19.1880
_cell_measurement_theta_min      3.1170
_cell_volume                     4356.5(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_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      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
  1 omega  -93.00   25.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3633    0.0000 -150.0000 118

  2 omega  -23.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.3633  -99.0000  -30.0000 45

  3 omega   35.00   79.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133  178.0000   90.0000 44

  4 omega    6.00   47.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133   57.0000  -90.0000 41

  5 omega  -42.00  -13.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133  -57.0000 -150.0000 29

  6 omega   -4.00   54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6133   37.0000  150.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0390692000
_diffrn_orient_matrix_UB_12      -0.0195381000
_diffrn_orient_matrix_UB_13      -0.0181018000
_diffrn_orient_matrix_UB_21      -0.0402054000
_diffrn_orient_matrix_UB_22      -0.0224528000
_diffrn_orient_matrix_UB_23      0.0035902000
_diffrn_orient_matrix_UB_31      -0.0207815000
_diffrn_orient_matrix_UB_32      0.0066708000
_diffrn_orient_matrix_UB_33      -0.0409496000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1797
_diffrn_reflns_av_unetI/netI     0.1658
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30081
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.303
_diffrn_reflns_theta_min         3.098
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.132
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull light green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_description       plate
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5929
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1731
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0210P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2707
_reflns_number_total             5929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00040b2.cif
_cod_data_source_block           koko786green
_cod_database_code               4349997
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'V2 C10 N4 O20 H10 Mo6 Cu2'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 H3SC-N3S
 0.85 with sigma of 0.01
 N3S-H3SD
 0.85 with sigma of 0.01
 N3S-H3SB = N3S-H3SA
 0.85 with sigma of 0.01
 O1S-H1SB = O1S-H1SA
 0.9 with sigma of 0.01
 H3SA-H3SB \\sim H3SB-H3SC
 with sigma of 0.01
 H3SA-H3SB \\sim H3SB-H3SD
 with sigma of 0.01
 H3SB-H3SD \\sim H3SD-H3SC
 with sigma of 0.01
 H3SD-H3SC \\sim H3SC-H3SB
 with sigma of 0.01
 H3SD-H3SC \\sim H3SC-H3SA
 with sigma of 0.01
 H3SA-H3SD \\sim H3SD-H3SB
 with sigma of 0.01
 H3SA-H3SD \\sim H3SD-H3SC
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6S) \\sim Ueq, Uanis(O7S) \\sim Ueq, Uanis(O4S) \\sim Ueq, Uanis(O5S)
\\sim Ueq, Uanis(O8S) \\sim Ueq, Uanis(O9S) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.03
4. Others
 Fixed Sof: O4S(0.75) H4SA(0.75) H4SB(0.75) O5S(0.25) H5SA(0.25) H5SB(0.25)
 O6S(0.3) H6SA(0.3) H6SB(0.3) O7S(0.7) H7SA(0.7) H7SB(0.7) O8S(0.07) H8SA(0.07)
 H8SB(0.07) O9S(0.35) H9SA(0.35) H9SB(0.35) O0AA(0.08) H0AA(0.08) H0AB(0.08)
5.a Riding coordinates:
 O1S(H1SA,H1SB), N3S(H3SA,H3SB,H3SC,H3SD), O4S(H4SA,H4SB), O5S(H5SA,H5SB),
 O6S(H6SA,H6SB), O7S(H7SA,H7SB), O8S(H8SA,H8SB), O9S(H9SA,H9SB), O0AA(H0AA,H0AB)
5.b Ternary CH refined with riding coordinates:
 N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), C1(H1C,H1D), C2(H2A,H2B), C3(H3C,H3D), C4(H4A,H4B)
;
_olex2_submission_original_sample_id koko786green
_olex2_submission_special_instructions 'No special instructions were received'