Cobalt-based molecular electrocatalysis of nitrile reduction: evolving sustainability beyond hydrogen.
Child, Simon N.; Raychev, Radoslav; Moss, Nathan; Howchen, Benjamin; Horton, Peter N.; Prior, Christopher C.; Oganesyan, Vasily S.; Fielden, John; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9576–9580; doi:10.1039/c9dt00773c

data_7700244
_publ_section_title
;
 Cobalt-based molecular electrocatalysis of nitrile reduction: evolving
 sustainability beyond hydrogen.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9576
_journal_page_last               9580
_journal_paper_doi               10.1039/c9dt00773c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H24 Co N4 O2, 2(N O3)'
_chemical_formula_sum            'C18 H24 Co N6 O8'
_chemical_formula_weight         511.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-02-20 deposited with the CCDC.    2019-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.734(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6698(4)
_cell_length_b                   10.05059(18)
_cell_length_c                   16.0714(4)
_cell_measurement_reflns_used    10976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5320
_cell_measurement_theta_min      2.5400
_cell_volume                     2116.27(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -103.00  77.00   1.00    5.00    --  -13.00   0.00  60.00  180
  2  \w    -74.00  23.00   1.00    5.00    --  -13.00 -72.00-180.00   97
  3  \w    -60.00  23.00   1.00    5.00    --  -13.00 -72.00   0.00   83
  4  \w    -22.00   5.00   1.00    5.00    --  -13.00  54.00 -60.00   27
  5  \w    -63.00 -43.00   1.00    5.00    --  -13.00  18.00-150.00   20
  6  \w   -103.00 -26.00   1.00    5.00    --  -13.00   0.00 -60.00   77
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0327674000
_diffrn_orient_matrix_UB_12      0.0117084000
_diffrn_orient_matrix_UB_13      -0.0478145000
_diffrn_orient_matrix_UB_21      0.0313231000
_diffrn_orient_matrix_UB_22      -0.0409557000
_diffrn_orient_matrix_UB_23      -0.0124392000
_diffrn_orient_matrix_UB_31      -0.0295844000
_diffrn_orient_matrix_UB_32      -0.0562754000
_diffrn_orient_matrix_UB_33      -0.0008631000
_diffrn_radiation_collimation    'confocal mirrors'
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13100
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.110
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.6210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2336
_reflns_number_total             2431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00773c2.cif
_cod_data_source_block           2016ncs0097
_cod_depositor_comments
'Adding full bibliography for 7700244--7700245.cif.'
_cod_database_code               7700244
_chemical_oxdiff_formula         'C18 H20 Co N6 O6'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N4)
Uanis(C1) = Uanis(C18)
Uanis(C2) = Uanis(C17)
Uanis(C3) = Uanis(C16)
Uanis(C4) = Uanis(C15)
Uanis(C5) = Uanis(C14)
3. Others
 Fixed Sof: N1(0.5) N2(0.5) N3(0.5) N4(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5)
 C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5)
 C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C13(0.5) H13(0.5)
 C14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5)
 H18(0.5)
4.a Rotating group:
 O1(H1A,H1B)
4.b Ternary CH refined with riding coordinates:
 C7(H7), C9(H9)
4.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18)
;
_shelx_res_checksum              16418
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-09
_olex2_date_sample_submission    2016-02-16
_olex2_submission_original_sample_id BH1-19
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.766