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_7061306
_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_absolute_configuration unk
_chemical_formula_moiety         'C26 H16 Co N4 O2, H2 O'
_chemical_formula_sum            'C26 H18 Co N4 O3'
_chemical_formula_weight         493.39
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_Int_Tables_number      152
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc28cv9t
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.3668(6)
_cell_length_b                   13.3668(6)
_cell_length_c                   20.7353(10)
_cell_measurement_reflns_used    3005
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.6340
_cell_measurement_theta_min      4.2330
_cell_volume                     3208.5(3)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0606
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9917
_diffrn_measured_fraction_theta_max 0.7570
_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     49.00  79.00   1.00   13.53    --   14.45 178.00  60.00   30
  2  \w    -43.00  34.00   1.00   13.53    --   14.45 -19.00   0.00   77
;
_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      0.0288829000
_diffrn_orient_matrix_UB_12      0.0604397000
_diffrn_orient_matrix_UB_13      -0.0054316000
_diffrn_orient_matrix_UB_21      0.0265322000
_diffrn_orient_matrix_UB_22      0.0095744000
_diffrn_orient_matrix_UB_23      0.0307421000
_diffrn_orient_matrix_UB_31      0.0471111000
_diffrn_orient_matrix_UB_32      -0.0025899000
_diffrn_orient_matrix_UB_33      -0.0139899000
_diffrn_radiation_collimation    0.3
_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  0.0213
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7912
_diffrn_reflns_theta_full        29.1513
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.816
_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_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.5320
_exptl_crystal_description       block
_exptl_crystal_F_000             1520.7218
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4149
_refine_diff_density_min         -0.2909
_refine_diff_density_rms         0.0577
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_d_res_high            0.7295
_refine_ls_d_res_low             5.9344
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0481
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0481
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.5886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.603
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              8
_reflns_limit_k_min              -7
_reflns_limit_l_max              28
_reflns_limit_l_min              -28
_reflns_number_gt                3640
_reflns_number_total             4371
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj06003a2.cif
_cod_data_source_block           CSB0
_cod_depositor_comments
'Adding full bibliography for 7061306--7061307.cif.'
_cod_original_sg_symbol_Hall     ' P 31 2"'
_cod_database_code               7061306
_chemical_oxdiff_usercomment     'MOD DIFF'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9994(4)
 0.0006(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3.a Free rotating group:
 O3(H3a,H3b)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C19(H19), C20(H20), C2(H2), C3(H3),
 C4(H4), C5(H5), C6(H6), C22(H22), C23(H23), C21(H21)
;
_olex2_date_sample_completion    2017-03-08
_olex2_date_sample_data_collection 2017-03-08
_olex2_date_sample_submission    2017-03-08
_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 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.739