Ligand-centered electrochemical processes enable CO2 reduction with a nickel bis(triazapentadienyl) complex
Dubrawski, Zachary; Heidebrecht, Joshua; Puerta Lombardi, Braulio M.; Hyla, Alexander S.; Willkomm, Janina; Radford, Chase L.; Lin, Jian-Bin; Welch, Gregory C.; Ponnurangam, Sathish; Roesler, Roland; Prokopchuk, Demyan E.; Piers, Warren E.; Sustainable Energy & Fuels 3 (2019) 1172–; doi:10.1039/C8SE00623G

data_1554614
_publ_section_title
;
 Ligand-centered electrochemical processes enable CO2 reduction with a
 nickel bis(triazapentadienyl) complex
;
_journal_issue                   5
_journal_name_full               'Sustainable Energy &amp; Fuels'
_journal_page_first              1172
_journal_paper_doi               10.1039/C8SE00623G
_journal_volume                  3
_journal_year                    2019
_chemical_formula_moiety         'C36 H44 K2 N10 O3'
_chemical_formula_sum            'C36 H44 K2 N10 O3'
_chemical_formula_weight         743.01
_chemical_name_common            KTAPPy
_chemical_properties_physical    Air-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-14 deposited with the CCDC.	2019-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.794(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3268(9)
_cell_length_b                   7.3620(3)
_cell_length_c                   22.2054(9)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      72.02
_cell_measurement_theta_min      3.80
_cell_volume                     3800.0(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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      173.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26482
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.179
_diffrn_reflns_theta_min         1.900
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1206 before and 0.0743 after correction. The Ratio of minimum to maximum transmission is 0.6890. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_recrystallization_method
'Vapor diffusion of pentane into a THF solution of the compound'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7388
_refine_ls_number_restraints     498
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1084P)^2^+0.5490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6046
_reflns_number_total             7388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8se00623g2.cif
_cod_data_source_block           new
_cod_database_code               1554614
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 K1, K2, O1, O2, O3, N1, H1, N2, N3, H3, N4, N5, N6, H6, N7, N8, H8, N9, N10,
 C1, C2, C3, C4, H4, C5, H5, C6, H6A, C7, H7, C8, C9, H9, C10, H10, C11, H11,
 C12, H12, C13, C14, C15, C16, H16, C17, H17, C18, H18, C19, H19, C20, C21, H21,
  C22, H22, C23, H23, C24, H24, C25, H25A, H25B, C26, H26A, H26B, C27, H27A,
 H27B, C28, H28A, H28B, C29, H29A, H29B, C30, H30A, H30B, C31, H31A, H31B, C32,
 H32A, H32B, C33, H33A, H33B, C34, H34A, H34B, C35, H35A, H35B, C36, H36A, H36B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3), N6(H6), N8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6A), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              79041
_shelx_hkl_checksum              51005
_olex2_submission_original_sample_id KTAPPy
_olex2_submission_special_instructions 'No special instructions were received'