Redox-Active Ligand Assisted Multielectron Catalysis: A Case of CoIII Complex as Water Oxidation Catalyst.
Du, Hao-Yi; Chen, Si-Cong; Su, Xiao-Jun; Jiao, Lei; Zhang, Ming-Tian; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.8b00032

data_4127073
_publ_section_title
;
 Redox-Active Ligand Assisted Multielectron Catalysis: A Case of CoIII
 Complex as Water Oxidation Catalyst.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.8b00032
_journal_year                    2018
_chemical_formula_moiety         'C22 H36 Co N4 Na O5, C1.5 O0.5'
_chemical_formula_sum            'C23.5 H36 Co N4 Na O5.5'
_chemical_formula_weight         544.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.493(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3649(14)
_cell_length_b                   10.2878(7)
_cell_length_c                   19.8168(16)
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    178.2(9)
_cell_measurement_theta_max      64.9090
_cell_measurement_theta_min      4.8530
_cell_volume                     2859.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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      178.2(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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    -69.00  38.00   1.00    1.52    --  -40.81  19.00-150.00  107
  2  \w     17.00 108.00   1.00    6.09    --   89.35 -61.00  90.00   91
  3  \w     68.00 153.00   1.00    6.09    --   89.35  45.00   0.00   85
  4  \w    133.00 160.00   1.00    6.09    --   89.35 125.00 120.00   27
  5  \w     65.00 162.00   1.00    6.09    --   89.35  45.00-120.00   97
  6  \w     96.00 148.00   1.00    6.09    --   89.35 125.00-180.00   52
  7  \w     70.00 106.00   1.00    6.09    --   89.35 -95.00 -90.00   36
  8  \w   -115.00 -34.00   1.00    1.52    --  -40.81 -38.00  30.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0629428000
_diffrn_orient_matrix_UB_12      -0.0892340000
_diffrn_orient_matrix_UB_13      -0.0537480000
_diffrn_orient_matrix_UB_21      0.0780436000
_diffrn_orient_matrix_UB_22      -0.0027318000
_diffrn_orient_matrix_UB_23      -0.0424232000
_diffrn_orient_matrix_UB_31      0.0447986000
_diffrn_orient_matrix_UB_32      -0.1203052000
_diffrn_orient_matrix_UB_33      0.0406180000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9816
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        65.714
_diffrn_reflns_theta_max         65.714
_diffrn_reflns_theta_min         4.571
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4825
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0914P)^2^+0.8041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3448
_reflns_number_total             4825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00032_si_003.cif
_cod_data_source_block           duhaoyi4
_cod_original_formula_sum        'C23.50 H36 Co N4 Na O5.50'
_cod_database_code               4127073
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1AA-O2AA
 1.258 with sigma of 0.02
 C1AA-C0AA
 1.54 with sigma of 0.02
 C0AA-O2AA
 2.43 with sigma of 0.02
3. Others
 Fixed Sof: C1AA(0.5) O2AA(0.5)
4.a Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C11(H11A,
 H11B,H11C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C),
 C21(H21A,H21B,H21C)
;
_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 3.378
_oxdiff_exptl_absorpt_empirical_full_min 0.464