Molecular Cobalt Complexes with Pendant Amines for Selective Electrocatalytic Reduction of Carbon Dioxide to Formic Acid.
Roy, Souvik; Sharma, Bhaskar; Pécaut, Jacques; Simon, Philippe; Fontecave, Marc; Tran, Phong D.; Derat, Etienne; Artero, Vincent; Journal of the American Chemical Society 139 (2017) 3685–3696; doi:10.1021/jacs.6b11474

data_4125620
_publ_section_title
;
 Molecular Cobalt Complexes with Pendant Amines for Selective
 Electrocatalytic Reduction of Carbon Dioxide to Formic Acid.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3685
_journal_page_last               3696
_journal_paper_doi               10.1021/jacs.6b11474
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'C34 H33 Co F3 N2 O3 P2 S, 0.39(C1 H2 Cl2), C F3 O3 S'
_chemical_formula_sum            'C35.38 H33.77 Cl0.77 Co F6 N2 O6 P2 S2'
_chemical_formula_weight         909.32
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                100.465(2)
_cell_angle_beta                 94.427(2)
_cell_angle_gamma                94.263(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1042(3)
_cell_length_b                   10.6408(3)
_cell_length_c                   20.6460(6)
_cell_measurement_reflns_used    5813
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9386
_cell_measurement_theta_min      3.3879
_cell_volume                     1952.98(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -11.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0769   77.0000  -60.0000 92

  2 omega  -49.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0769  -77.0000 -180.0000 95

  3 omega   34.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0769   37.0000  120.0000 54

  4 omega  -45.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8738   77.0000   30.0000 91
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0071153000
_diffrn_orient_matrix_UB_12      0.0043810000
_diffrn_orient_matrix_UB_13      0.0342900000
_diffrn_orient_matrix_UB_21      0.0410351000
_diffrn_orient_matrix_UB_22      0.0609754000
_diffrn_orient_matrix_UB_23      0.0065981000
_diffrn_orient_matrix_UB_31      -0.0664956000
_diffrn_orient_matrix_UB_32      0.0299223000
_diffrn_orient_matrix_UB_33      -0.0034263000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12773
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.200
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.395
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.381
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         7900
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0626P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5308
_reflns_number_total             7900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11474_si_005.cif
_cod_data_source_block           p281
_cod_depositor_comments
'Adding full bibliography for 4125618--4125621.cif.'
_cod_original_cell_volume        1952.99(10)
_cod_database_code               4125620
_chemical_oxdiff_formula         'Co I N2 C35 H35 P2 S2 O6 F6'
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.686
_reflns_odcompleteness_completeness 98.86
_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
2. Uiso/Uaniso restraints and constraints
C20B \\sim C20 \\sim C19 \\sim C19B \\sim C18B \\sim C18 \\sim C17 \\sim C17B
\\sim C22 \\sim C22B \\sim C21 \\sim C21B: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=
 Sof(H21B)=Sof(C17B)=Sof(C22B)=Sof(H22B)=1-FVAR(1)
 Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(H22)=FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C41(H41A,H41B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C18B(H18B), C19B(H19B), C20B(H20B), C21B(H21B), C22B(H22B), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'