Hybrid compound based on diethylenetriaminecopper(ii) cations and scarce V-monosubstituted β-octamolybdate as water oxidation catalyst
Buvailo, Halyna I.; Makhankova, Valeriya G.; Kokozay, Vladimir N.; Omelchenko, Iryna V.; Shishkina, Svitlana V.; Bieńko, Alina; Pavliuk, Mariia V.; Shylin, Sergii I.; RSC Advances 11 (2021) 32119–32125; doi:10.1039/D1RA05030C

data_7243641
_publ_section_title
;
 Hybrid compound based on diethylenetriaminecopper(ii) cations and scarce
 V-monosubstituted \b-octamolybdate as water oxidation catalyst
;
_journal_issue                   51
_journal_name_full               'RSC Advances'
_journal_page_first              32119
_journal_page_last               32125
_journal_paper_doi               10.1039/D1RA05030C
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety
'Mo7 O26 V, 0.5(H8 N2), 2(C4 H17 Cu N3 O2), 1.5(H2 O)'
_chemical_formula_sum            'C8 H41 Cu2 Mo7 N7 O31.5 V'
_chemical_formula_weight         1589.08
_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             2018-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-10-11 deposited with the CCDC.	2021-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.260(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8374(5)
_cell_length_b                   13.8773(7)
_cell_length_c                   14.1652(8)
_cell_measurement_reflns_used    2051
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.5150
_cell_measurement_theta_min      3.2580
_cell_volume                     1930.65(18)
_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 0.996
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega  -66.00    4.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5425  -77.0000  150.0000 70

  2 omega  -24.00   63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7925  -99.0000  -60.0000 87

  3 omega   39.00   89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7925   57.0000   90.0000 50

  4 omega  -40.00   28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7925  -19.0000  -30.0000 68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0425700000
_diffrn_orient_matrix_UB_12      -0.0258787000
_diffrn_orient_matrix_UB_13      0.0332118000
_diffrn_orient_matrix_UB_21      0.0562234000
_diffrn_orient_matrix_UB_22      0.0076424000
_diffrn_orient_matrix_UB_23      -0.0282745000
_diffrn_orient_matrix_UB_31      0.0154509000
_diffrn_orient_matrix_UB_32      0.0434082000
_diffrn_orient_matrix_UB_33      0.0247983000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12738
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         32.480
_diffrn_reflns_theta_min         3.233
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    3.609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47188
_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            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_description       block
_exptl_crystal_F_000             1530
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.983
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+3.8427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4122
_reflns_number_total             6128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra05030c2.cif
_cod_data_source_block           koko805
_cod_original_cell_volume        1930.65(17)
_cod_original_formula_sum        'C8 H41 Cu2 Mo7 N7 O31.50 V'
_cod_database_code               7243641
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.78
_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. Shared sites
{V1, Mo1}
3. Uiso/Uaniso restraints and constraints
Uanis(V1) = Uanis(Mo1)
4. Others
 Fixed Sof: Mo1(0.5) V1(0.5) H1SC(0.5) H1SD(0.5) H1SE(0.5) H1SF(0.5) O3S(0.75)
 H3SA(0.75) H3SB(0.75)
5.a Riding coordinates:
 N1S(H1SC,H1SD,H1SE,H1SF), O1S(H1SA,H1SB), O2S(H2SA,H2SB), O3S(H3SA,H3SB)
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_date_sample_data_collection 2017-04-27
_olex2_submission_original_sample_id koko805
_olex2_submission_special_instructions 'No special instructions were received'