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_4125621
_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         'C35 H48 Co N3 P2, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C39 H51 Co F6 N4 O6 P2 S2'
_chemical_formula_weight         970.82
_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   difmap
_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                100.479(4)
_cell_angle_beta                 103.371(4)
_cell_angle_gamma                102.291(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0634(5)
_cell_length_b                   11.8443(5)
_cell_length_c                   18.1779(8)
_cell_measurement_reflns_used    5700
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.3960
_cell_measurement_theta_min      2.3720
_cell_volume                     2196.38(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   -4.00   96.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   77.0000 -120.0000 100

  2 omega  -25.00   67.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000  120.0000 92

  3 omega  -25.00   67.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000    0.0000 92

  4 omega -100.00   46.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9676    0.0000  -90.0000 146

  5 omega    4.00   62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   56.0000  130.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0252600000
_diffrn_orient_matrix_UB_12      0.0447724000
_diffrn_orient_matrix_UB_13      -0.0139747000
_diffrn_orient_matrix_UB_21      -0.0562646000
_diffrn_orient_matrix_UB_22      -0.0440782000
_diffrn_orient_matrix_UB_23      -0.0239364000
_diffrn_orient_matrix_UB_31      -0.0295092000
_diffrn_orient_matrix_UB_32      0.0067059000
_diffrn_orient_matrix_UB_33      0.0306821000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26717
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense red'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         13328
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0380P)^2^+0.6041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9438
_reflns_number_total             13328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b11474_si_003.cif
_cod_data_source_block           sr2015_18
_cod_depositor_comments
'Adding full bibliography for 4125618--4125621.cif.'
_cod_original_cell_volume        2196.38(17)
_cod_database_code               4125621
_chemical_oxdiff_formula         'C36 H51 Co N3 P2 S2 F6 O6'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.862
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq, Uanis(C2SB) \\sim Ueq, Uanis(F6S2) \\sim Ueq, Uanis(F3S2)
\\sim Ueq, Uanis(F2S2) \\sim Ueq, Uanis(F5S2) \\sim Ueq, Uanis(F4S2) \\sim Ueq,
Uanis(F1S2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
2. Others
 Sof(F4S2)=Sof(F5S2)=Sof(F6S2)=Sof(C2SB)=1-FVAR(1)
 Sof(F1S2)=Sof(F2S2)=Sof(F3S2)=Sof(C2S)=FVAR(1)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'