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_1554615
_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         'C24 H20 N10 Ni'
_chemical_formula_sum            'C24 H20 N10 Ni'
_chemical_formula_weight         507.21
_chemical_name_common            Ni(TAPPy)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-01
_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                 101.096(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7492(13)
_cell_length_b                   16.392(2)
_cell_length_c                   8.8505(14)
_cell_measurement_reflns_used    1314
_cell_measurement_temperature    173
_cell_measurement_theta_max      20.30
_cell_measurement_theta_min      2.95
_cell_volume                     1103.2(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14166
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         3.436
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0689 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.8682.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF;Hexanes'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0253P)^2^+0.7669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1542
_reflns_number_total             2158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8se00623g2.cif
_cod_data_source_block           180727zack_0m_a
_cod_database_code               1554615
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Riding coordinates:
 N1(H1), N3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              73391
_shelx_hkl_checksum              3477
_olex2_submission_special_instructions 'No special instructions were received'