Electrochemical CO2 reduction by a cobalt bipyricorrole complex: Decrease of an overpotential value derived from monoanionic ligand character of the porphyrinoid species
Ogawa, Ayumu; Oohora, Koji; Gu, Wenting; Hayashi, Takashi; Chemical Communications  (2018) –; doi:10.1039/C8CC08876D

data_7122706
_publ_section_title
;
 Electrochemical CO2 reduction by a cobalt bipyricorrole complex: Decrease
 of an overpotential value derived from monoanionic ligand character of
 the porphyrinoid species
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08876D
_journal_year                    2018
_chemical_formula_moiety         'C38 H41 Co N4 O3, Cl O4'
_chemical_formula_sum            'C38 H41 Cl Co N4 O7'
_chemical_formula_weight         760.16
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-01 deposited with the CCDC.
2018-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.558(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1338(7)
_cell_length_b                   28.115(2)
_cell_length_c                   12.8255(9)
_cell_measurement_reflns_used    5772
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      70.4410
_cell_measurement_theta_min      3.9270
_cell_volume                     3520.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9620
_diffrn_measured_fraction_theta_max 0.9612
_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     69.00 105.00   0.50   24.57    --   42.80  77.00-150.00   72
  2  \w     85.00 110.00   0.50   98.29    --   76.50 129.00-157.00   50
  3  \w     88.00 116.00   0.50   24.57    --   42.80 125.00 -90.00   56
  4  \w     64.00  89.00   0.50   24.57    --   42.80 141.00  15.00   50
  5  \w     81.00 106.00   0.50   98.29    --   76.50 141.00  15.00   50
  6  \w     15.00  65.00   0.50   24.57    --   42.80  77.00-150.00  100
  7  \w    -82.00 -55.00   0.50   24.57    --  -42.80 129.00-157.00   54
  8  \w     43.00  68.00   0.50   98.29    --   76.50-129.00 129.00   50
  9  \w     31.00  56.00   0.50   98.29    --   76.50-141.00 -43.00   50
 10  \w   -112.00 -87.00   0.50   24.57    --  -42.80-141.00 -43.00   50
 11  \w   -116.00 -71.00   0.50   24.57    --  -42.80-125.00 -30.00   90
 12  \w   -116.00 -72.00   0.50   24.57    --  -42.80-125.00-150.00   88
 13  \w   -115.00 -70.00   0.50   24.57    --  -42.80-125.00-180.00   90
 14  \w   -177.00 -81.00   0.50   98.29    -- -106.00-125.00   0.00  192
 15  \w   -127.00-101.00   0.50   98.29    -- -106.00-129.00 129.00   52
 16  \w   -131.00-105.00   0.50   98.29    -- -106.00 -37.00 120.00   52
 17  \w   -166.00 -78.00   0.50   98.29    -- -106.00-125.00  30.00  176
 18  \w   -176.00 -96.00   0.50   98.29    -- -106.00 -57.00  60.00  160
 19  \w   -177.00-142.00   0.50   98.29    -- -106.00 -37.00 120.00   70
 20  \w   -177.00 -85.00   0.50   98.29    -- -106.00 -57.00  30.00  184
 21  \w    -53.00 -28.00   0.50   98.29    -- -106.00  37.00 -90.00   50
 22  \w    -73.00 -46.00   0.50   98.29    -- -106.00  57.00-150.00   54
 23  \w    -84.00 -43.00   0.50   98.29    -- -106.00  57.00-120.00   82
 24  \w    -71.00 -46.00   0.50   98.29    -- -106.00 125.00-150.00   50
 25  \w   -103.00 -77.00   0.50   98.29    -- -106.00 125.00 -30.00   52
 26  \w    -79.00 -41.00   0.50   98.29    -- -106.00 141.00  15.00   76
 27  \w    -57.00 -32.00   0.50   98.29    -- -106.00 125.00  60.00   50
 28  \w   -102.00 -77.00   0.50   98.29    -- -106.00 125.00  60.00   50
 29  \w   -129.00 -82.00   0.50   98.29    -- -106.00 141.00  15.00   94
 30  \w   -120.00 -52.00   0.50   98.29    -- -106.00 125.00 -60.00  136
 31  \w   -105.00 -53.00   0.50   24.57    --  -42.80 141.00  15.00  104
 32  \w   -120.00 -95.00   0.50   98.29    -- -106.00  57.00-120.00   50
 33  \w   -128.00 -95.00   0.50   98.29    -- -106.00  57.00-150.00   66
 34  \w   -120.00 -76.00   0.50   98.29    -- -106.00 129.00-157.00   88
 35  \w   -118.00 -41.00   0.50   98.29    -- -106.00 125.00-180.00  154
 36  \w   -175.00-112.00   0.50   98.29    -- -106.00-125.00-180.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0215312000
_diffrn_orient_matrix_UB_12      -0.0531217000
_diffrn_orient_matrix_UB_13      0.0292063000
_diffrn_orient_matrix_UB_21      0.0607111000
_diffrn_orient_matrix_UB_22      0.0133002000
_diffrn_orient_matrix_UB_23      0.1198333000
_diffrn_orient_matrix_UB_31      -0.1440435000
_diffrn_orient_matrix_UB_32      -0.0022951000
_diffrn_orient_matrix_UB_33      0.0181994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1664
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30554
_diffrn_reflns_theta_full        75.6205
_diffrn_reflns_theta_max         75.62
_diffrn_reflns_theta_min         3.91
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.4342
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584.5880
_exptl_crystal_recrystallization_method 'H2O/CH3OH = 1/4'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.1955
_refine_diff_density_min         -0.9609
_refine_diff_density_rms         0.1835
_refine_ls_d_res_high            0.7959
_refine_ls_d_res_low             11.3114
_refine_ls_goodness_of_fit_ref   1.0219
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7034
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0216
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2544
_refine_ls_wR_factor_ref         0.3097
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4032
_reflns_number_total             7034
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8cc08876d2.cif
_cod_data_source_block           CoBIPC_1
_cod_database_code               7122706
_chemical_oxdiff_formula         'C37 H37 N4 O6 Cl Co'
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 C8-H7
 1.956431 with sigma of 0.02
 Co1-H7
 2.852815 with sigma of 0.02
3. Others
 Sof(C40a)=Sof(H40c)=Sof(H40d)=Sof(C41a)=Sof(H41d)=Sof(H41e)=Sof(H41f)=1-FVAR(1)
 Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(H41c)=FVAR(1)
 Sof(Cl1a)=Sof(O2a)=Sof(O0ab)=Sof(O3a)=1-FVAR(2)
 Sof(Cl1)=Sof(O0aa)=Sof(O2)=Sof(O3)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C48(H48a,H48b), C37(H37a,H37b), C50(H50a,H50b), C40(H40a,H40b), C40a(H40c,H40d)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C12(H12), C19(H19), C11(H11), C21(H21), C42(H42), C18(H18),
 C13(H13), C28(H28), C33(H33), C29(H29)
4.c Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C35(H35a,H35b,H35c), C49(H49a,H49b,H49c), C8(H8a,H8b,
 H8c), C51(H51a,H51b,H51c), C32(H32a,H32b,H32c), C41(H41a,H41b,H41c), C41a(H41d,
 H41e,H41f)
;
_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 3.174
_oxdiff_exptl_absorpt_empirical_full_min 0.309