Immobilization of “Capping Arene” Cobalt(II) Complexes on Ordered Mesoporous Carbon for Electrocatalytic Water Oxidation
Liu, Chang; Geer, Ana M.; Webber, Christopher; Musgrave, Charles B.; Gu, Shunyan; Johnson, Grayson; Dickie, Diane A.; Chabbra, Sonia; Schnegg, Alexander; Zhou, Hua; Sun, Cheng-Jun; Hwang, Sooyeon; Goddard, William A.; Zhang, Sen; Gunnoe, T. Brent; ACS Catalysis 11 (2021) 15068–15082; doi:10.1021/acscatal.1c04617

data_4519245
_publ_section_title
;
 Immobilization of &#x201C;Capping Arene&#x201D; Cobalt(II) Complexes on
 Ordered Mesoporous Carbon for Electrocatalytic Water Oxidation
;
_journal_issue                   24
_journal_name_full               'ACS Catalysis'
_journal_page_first              15068
_journal_page_last               15082
_journal_paper_doi               10.1021/acscatal.1c04617
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C24 H16 Co N4 O6, C H2 Cl2'
_chemical_formula_sum            'C25 H18 Cl2 Co N4 O6'
_chemical_formula_weight         600.26
_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     direct
_audit_creation_date             2020-09-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.257(2)
_cell_angle_beta                 105.396(2)
_cell_angle_gamma                99.442(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2834(6)
_cell_length_b                   9.3346(6)
_cell_length_c                   15.0022(10)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.803
_cell_measurement_theta_min      2.217
_cell_volume                     1233.47(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service v2017.5.0.0'
_computing_data_reduction        'SAINT V8.40A (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            70953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.529
_diffrn_reflns_theta_min         1.411
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0515 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.9228.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0282P)^2^+0.6635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6306
_reflns_number_total             7545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c04617_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               4519245
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Others
 Sof(H25C)=Sof(H25D)=Sof(Cl1A)=Sof(Cl2A)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25(H25C,H25D)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              94251
_shelx_hkl_checksum              49272