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_4349995
_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
'Mo6 O26 V2, C4 H16 Cu N4, C2 H10 N2, 2(H4 N), 4(H2 O)'
_chemical_formula_sum            'C6 H42 Cu Mo6 N8 O30 V2'
_chemical_formula_weight         1447.53
_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
_atom_sites_solution_primary     direct
_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                102.267(4)
_cell_angle_beta                 112.333(5)
_cell_angle_gamma                99.415(5)
_cell_formula_units_Z            1
_cell_length_a                   8.5468(5)
_cell_length_b                   10.9507(5)
_cell_length_c                   10.9914(4)
_cell_measurement_reflns_used    2913
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.6810
_cell_measurement_theta_min      3.7250
_cell_volume                     895.22(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 0.997
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details
;
  1 omega -102.00  -50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583  178.0000   30.0000 52

  2 omega   10.00   40.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583   77.0000  120.0000 30

  3 omega  -92.00    0.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583  -77.0000    0.0000 92

  4 omega  -53.00  -27.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583   77.0000  120.0000 26

  5 omega    7.00   65.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6083  -99.0000 -120.0000 58

  6 omega   -5.00   29.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6083   89.0000  -17.0000 34

  7 omega  -36.00  100.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6083    0.0000  -30.0000 136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0782400000
_diffrn_orient_matrix_UB_12      -0.0164022000
_diffrn_orient_matrix_UB_13      0.0036244000
_diffrn_orient_matrix_UB_21      0.0307574000
_diffrn_orient_matrix_UB_22      0.0602799000
_diffrn_orient_matrix_UB_23      -0.0086954000
_diffrn_orient_matrix_UB_31      0.0402071000
_diffrn_orient_matrix_UB_32      0.0289388000
_diffrn_orient_matrix_UB_33      0.0725481000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9455
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.366
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63594
_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 light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.685
_exptl_crystal_description       plate
_exptl_crystal_F_000             701
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0057P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3921
_reflns_number_total             5609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00040b2.cif
_cod_data_source_block           koko663
_cod_original_cell_volume        895.21(8)
_cod_database_code               4349995
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.87
_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,H) groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O15B) \\sim Ueq, Uanis(O15A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: H3AA(0.6) H3AB(0.6) H3AC(0.6) H3BD(0.4) H3BE(0.4) H3BF(0.4)
 C3A(0.4) H3AD(0.4) H3AE(0.4) C3B(0.6) H3BA(0.6) H3BB(0.6) O15B(0.45)
 H15A(0.45) H15B(0.45) O15A(0.55) H15C(0.55) H15D(0.55)
4.a Riding coordinates:
 N4(H4A,H4B,H4C,H4D), O15B(H15A,H15B), O15A(H15C,H15D)
4.b Free rotating group:
 O14(H14A,H14B)
4.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3A(H3AD,H3AE), C3B(H3BA,
 H3BB)
4.d Me refined with riding coordinates:
 N3(H3AA,H3AB,H3AC), N3(H3BD,H3BE,H3BF)
;
_olex2_date_sample_data_collection 2015-10-05
_olex2_date_sample_submission    2015-10-01
_olex2_submission_original_sample_id koko663
_olex2_submission_special_instructions 'No special instructions were received'