Redox-inactive metal single-site molecular complexes: a new generation of electrocatalysts for oxygen evolution?
Benkó, Tímea; Lukács, Dávid; Frey, Krisztina; Németh, Miklós; Móricz, Márta M.; Liu, Dongyu; Kováts, Éva; May, Nóra V.; Vayssieres, Lionel; Li, Mingtao; Pap, József S.; Catalysis Science & Technology 11 (2021) 6411–6424; doi:10.1039/D1CY01087E

data_1564378
_publ_section_title
;
 Redox-inactive metal single-site molecular complexes: a new generation of
 electrocatalysts for oxygen evolution?
;
_journal_issue                   19
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6411
_journal_page_last               6424
_journal_paper_doi               10.1039/D1CY01087E
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety
'C55 H36 Cu3 N15 O3, Cl O4, C H4 O'
_chemical_formula_sum            'C56 H41 Cl Cu3 N15 O8'
_chemical_formula_weight         1278.10
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-01 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                76.118(2)
_cell_angle_beta                 87.983(2)
_cell_angle_gamma                82.560(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4454(3)
_cell_length_b                   13.2667(4)
_cell_length_c                   16.8433(5)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      76.1560
_cell_measurement_theta_min      4.4650
_cell_volume                     2677.01(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5908
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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    -67.00  36.00   1.00    1.00    --  -40.19  38.00 150.00  103
  2  \w    -74.00  39.00   1.00    1.00    --  -40.19  77.00-150.00  113
  3  \w   -116.00 -14.00   1.00    1.00    --  -40.19 -38.00 -30.00  102
  4  \w    -86.00  -6.00   1.00    1.00    --  -40.19 125.00-120.00   80
  5  \w      4.00  31.00   1.00    1.00    --   40.19  86.00  26.69   27
  6  \w     35.00 109.00   1.00    3.00    --  113.00-111.00-150.00   74
  7  \w     45.00  74.00   1.00    3.00    --  113.00-111.00-120.00   29
  8  \w     50.00 146.00   1.00    3.00    --  113.00 -77.00 -90.00   96
  9  \w     93.00 174.00   1.00    3.00    --  113.00  61.00 -60.00   81
 10  \w     75.00 109.00   1.00    3.00    --  113.00-111.00 -60.00   34
 11  \w    105.00 176.00   1.00    3.00    --  113.00 111.00   0.00   71
 12  \w     36.00  63.00   1.00    3.00    --  113.00-111.00 -60.00   27
 13  \w     83.00 109.00   1.00    3.00    --  113.00-111.00-120.00   26
 14  \w     35.00 107.00   1.00    3.00    --  113.00-111.00-180.00   72
 15  \w     84.00 170.00   1.00    3.00    --  113.00  61.00   0.00   86
 16  \w     84.00 177.00   1.00    3.00    --  113.00  55.00  58.57   93
 17  \w     59.00 109.00   1.00    3.00    --  113.00-111.00  90.00   50
 18  \w    104.00 178.00   1.00    3.00    --  113.00 111.00-120.00   74
 19  \w     37.00  78.00   1.00    3.00    --  113.00-111.00 120.00   41
 20  \w     84.00 109.00   1.00    3.00    --  113.00-111.00 120.00   25
 21  \w     83.00 170.00   1.00    3.00    --  113.00  61.00 -30.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0859877000
_diffrn_orient_matrix_UB_12      0.0925276000
_diffrn_orient_matrix_UB_13      0.0059457000
_diffrn_orient_matrix_UB_21      0.0670700000
_diffrn_orient_matrix_UB_22      0.0241020000
_diffrn_orient_matrix_UB_23      0.0668137000
_diffrn_orient_matrix_UB_31      0.0607640000
_diffrn_orient_matrix_UB_32      0.0734312000
_diffrn_orient_matrix_UB_33      -0.0661625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21558
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.307
_diffrn_reflns_theta_min         3.459
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         10968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0516P)^2^+0.9383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9276
_reflns_number_total             10968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy01087e2.cif
_cod_data_source_block           exp_1057
_cod_depositor_comments
;
Adding full bibliography for 1564378--1564379.cif.

2022-06-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         639.05
_cod_original_formula_moiety
'0.5(C55 H36 Cu3 N15 O3), 0.5(Cl O4), 0.5(C H4 O)'
_cod_original_formula_units_Z            4
_cod_original_formula_sum        'C28 H20.50 Cl0.50 Cu1.50 N7.50 O4'
_cod_database_code               1564378
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu2 C18 N10 O4'
_chemical_oxdiff_usercomment     'PJ2021/1: Cu2Ind #1 ujra'
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.640
_diffrn_oxdiff_digest_frames
;
01bc789f0f6c451dfdb48647a92c5614740139136dc
;
_diffrn_oxdiff_digest_hkl
;
012eb0f8029f7853092feddbce87ae9e6c56d7
;
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C19(H19), C22(H22), C23(H23), C25(H25), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
2.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              56975
_shelx_fab_checksum              85101
_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 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.835