Copper(II) defect-cubane water oxidation electrocatalysts: from molecular tetramers to oxidic nanostructures.
Adiyeri Saseendran, Devi Prasad; Fischer, Jörg W A; Müller, Lea; Abbott, Daniel F.; Mougel, Victor; Jeschke, Gunnar; Triana, Carlos A.; Patzke, Greta R.; Chemical communications (Cambridge, England) 59 (2023) 5866–5869; doi:10.1039/d3cc01005h

data_7131586
_publ_section_title
;
 Copper(II) defect-cubane water oxidation electrocatalysts: from molecular
 tetramers to oxidic nanostructures.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5866
_journal_page_last               5869
_journal_paper_doi               10.1039/d3cc01005h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C20 H30 Cu2 N2 O8, 2(H2 O)'
_chemical_formula_sum            'C20 H34 Cu2 N2 O10'
_chemical_formula_weight         589.57
_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     dual
_audit_creation_date             2022-10-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-27 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                71.0760(10)
_cell_angle_beta                 86.2810(10)
_cell_angle_gamma                77.2790(10)
_cell_formula_units_Z            1
_cell_length_a                   8.02330(10)
_cell_length_b                   8.8028(2)
_cell_length_c                   9.65090(10)
_cell_measurement_reflns_used    36194
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      37.9080
_cell_measurement_theta_min      2.4940
_cell_volume                     628.935(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_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  45.00   0.50    2.50    --   14.35  57.00  30.00   86
  2  \w      9.00  74.00   0.50    2.50    --   14.35  57.00 150.00  130
  3  \w     16.00  80.00   0.50    2.50    --   14.35  57.00  60.00  128
  4  \w     24.00  82.00   0.50    2.50    --   14.35  19.00-180.00  116
  5  \w      0.00  27.00   0.50    2.50    --   14.35 -57.00-180.00   54
  6  \w    -84.00  -1.00   0.50    2.50    --  -15.76 -59.00-140.56  166
  7  \w    -90.00 -12.00   0.50    2.50    --  -15.76 -19.00 -60.00  156
  8  \w    -94.00  -7.00   0.50    2.50    --  -15.76 -19.00-150.00  174
  9  \w    -42.00  -8.00   0.50    2.50    --  -15.76 -57.00   0.00   68
 10  \w    -60.00  -2.00   0.50    2.50    --  -15.76 -57.00 120.00  116
 11  \w    -45.00 -19.00   0.50    2.50    --  -15.76 -60.00 -59.31   52
 12  \w    -31.00  32.00   0.50    2.50    --  -15.76  60.00 153.76  126
 13  \w    -31.00  -6.00   0.50    2.50    --  -15.76  60.00-163.40   50
 14  \w      2.00  33.00   0.50    2.50    --  -15.76  60.00-163.40   62
 15  \w    -31.00  23.00   0.50    2.50    --  -15.76  60.00-117.52  108
 16  \w    -30.00  30.00   0.50    2.50    --  -15.76  57.00 -30.00  120
 17  \w    -30.00  37.00   0.50    2.50    --  -15.76  57.00   0.00  134
 18  \w    -30.00  28.00   0.50    2.50    --  -15.76  57.00 -90.00  116
 19  \w    -30.00  50.00   0.50    2.50    --  -15.76  57.00  30.00  160
 20  \w    -30.00  19.00   0.50    2.50    --  -15.76  57.00 -60.00   98
 21  \w    -30.00  41.00   0.50    2.50    --  -15.76  57.00 120.00  142
 22  \w    -30.00  31.00   0.50    2.50    --  -15.76  57.00  75.86  122
 23  \w     12.00  37.00   0.50    2.50    --   22.00 -60.00 -56.31   50
 24  \w    -94.00 -10.00   0.50    2.50    --  -22.09 -58.00 -78.21  168
 25  \w     -6.00  28.00   0.50    2.50    --  -22.09  57.00   0.00   68
 26  \w    -71.00 -14.00   0.50    2.50    --  -22.09 -60.00   4.16  114
 27  \w    -94.00 -48.00   0.50    2.50    --  -22.09 -59.00  32.97   92
 28  \w    -45.00  -9.00   0.50    2.50    --  -22.09 -59.00  32.97   72
 29  \w    -37.00  38.00   0.50    2.50    --  -22.09  60.00  69.65  150
 30  \w    -36.00  46.00   0.50    2.50    --  -22.09  57.00 -90.00  164
 31  \w    -89.00 -14.00   0.50    2.50    --  -22.09 -57.00-180.00  150
 32  \w    -36.00   1.00   0.50    2.50    --  -22.09  57.00-180.00   74
 33  \w      4.00  42.00   0.50    2.50    --  -22.09  57.00-180.00   76
 34  \w    -84.00 -16.00   0.50    2.50    --  -22.09 -57.00 120.00  136
 35  \w    -36.00  36.00   0.50    2.50    --  -22.09  57.00 150.00  144
 36  \w    -36.00 -10.00   0.50    2.50    --  -22.09  57.00   0.00   52
 37  \w    -93.00  -7.00   0.50    2.50    --  -22.09 -60.00-136.64  172
 38  \w    -36.00  12.00   0.50    2.50    --  -22.09  57.00 120.00   96
 39  \w    -36.00  50.00   0.50    2.50    --  -22.09  57.00 -60.00  172
 40  \w    -36.00  32.00   0.50    2.50    --  -22.09  57.00  30.00  136
 41  \w    -37.00  23.00   0.50    2.50    --  -22.09  60.00-141.55  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0590069000
_diffrn_orient_matrix_UB_12      -0.0297830000
_diffrn_orient_matrix_UB_13      0.0592542000
_diffrn_orient_matrix_UB_21      -0.0645329000
_diffrn_orient_matrix_UB_22      0.0271209000
_diffrn_orient_matrix_UB_23      0.0456216000
_diffrn_orient_matrix_UB_31      -0.0238279000
_diffrn_orient_matrix_UB_32      -0.0772736000
_diffrn_orient_matrix_UB_33      0.0210808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58956
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.921
_diffrn_reflns_theta_min         2.231
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         6442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0347P)^2^+0.1140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5683
_reflns_number_total             6442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01005h2.cif
_cod_data_source_block           Cu2(pyalk)2(OAc)2
_cod_depositor_comments
'Adding full bibliography for 7131586--7131587.cif.'
_cod_database_code               7131586
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H15 Cu N O5'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C3(H3), C2(H2)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              3877
_shelx_hkl_checksum              25276
_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 1.219
_oxdiff_exptl_absorpt_empirical_full_min 0.880