Electrocatalytic proton reduction by dinuclear cobalt complexes in a nonaqueous electrolyte
Raj, Manaswini; Padhi, Sumanta Kumar; New Journal of Chemistry 46 (2022) 6027–6038; doi:10.1039/D1NJ06003A

data_7061307
_publ_section_title
;
 Electrocatalytic proton reduction by dinuclear cobalt complexes in a
 nonaqueous electrolyte
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6027
_journal_page_last               6038
_journal_paper_doi               10.1039/D1NJ06003A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C54 H36 Co2 N8 O4, 5(H2 O), 1.75(O)'
_chemical_formula_sum            'C54 H49.5 Co2 N8 O10.75'
_chemical_formula_weight         1099.72
_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_block_doi                 10.5517/ccdc.csd.cc28cvbv
_audit_creation_date             2021-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2022-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.410(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9630(8)
_cell_length_b                   15.6404(8)
_cell_length_c                   25.9135(14)
_cell_measurement_reflns_used    6008
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8990
_cell_measurement_theta_min      2.3210
_cell_volume                     5150.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0303
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_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    -12.00  76.00   1.00  135.00    --   13.76  19.00 -60.00   88
  2  \w    -41.00  50.00   1.00  135.00    --  -15.95   0.00-150.00   91
  3  \w    -72.00 -36.00   1.00  135.00    --  -15.95-178.00 -30.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221849000
_diffrn_orient_matrix_UB_12      -0.0207391000
_diffrn_orient_matrix_UB_13      0.0195722000
_diffrn_orient_matrix_UB_21      0.0505335000
_diffrn_orient_matrix_UB_22      -0.0153535000
_diffrn_orient_matrix_UB_23      0.0120612000
_diffrn_orient_matrix_UB_31      0.0083872000
_diffrn_orient_matrix_UB_32      0.0372614000
_diffrn_orient_matrix_UB_33      0.0158754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        24.744
_diffrn_reflns_theta_max         24.744
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         8459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0985P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5801
_reflns_number_total             8459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj06003a2.cif
_cod_data_source_block           co_sbtol
_cod_depositor_comments
'Adding full bibliography for 7061306--7061307.cif.'
_cod_database_code               7061307
_chemical_oxdiff_formula         'C H N O Co'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O11(0.75)
3.a Free rotating group:
 O9(H9A,H9B), O6(H6A,H6B), O8(H8A,H8B), O7(H7A,H7B), O5(H5A,H5B)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C5(H5), C6(H6), C20(H20), C4(H4), C12(H12), C46(H46), C2(H2),
 C15(H15), C45(H45), C3(H3), C49(H49), C21(H21), C14(H14), C47(H47), C23(H23),
 C41(H41), C48(H48), C30(H30), C28(H28), C32(H32), C31(H31), C22(H22), C29(H29),
  C38(H38), C40(H40)
3.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_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 1.795
_oxdiff_exptl_absorpt_empirical_full_min 0.848