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_1554613
_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
'0.5(C24 H20 N10 Ni), 0.5(C18 H36 K N2 O6), 0.25(C6)'
_chemical_formula_sum            'C22.5 H28 K0.5 N6 Ni0.5 O3'
_chemical_formula_weight         479.41
_chemical_name_common            '[K(crypt)][Ni(TAPPy)2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-13
_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                78.667(5)
_cell_angle_beta                 85.315(5)
_cell_angle_gamma                77.907(5)
_cell_formula_units_Z            4
_cell_length_a                   12.9939(11)
_cell_length_b                   13.5751(15)
_cell_length_c                   14.0727(15)
_cell_measurement_reflns_used    5344
_cell_measurement_temperature    173
_cell_measurement_theta_max      20.4585
_cell_measurement_theta_min      2.7455
_cell_volume                     2377.8(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0900
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53862
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.123
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0684 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.8420.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             1010
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF:Hexanes'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         8346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0257P)^2^+3.8954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1227
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5720
_reflns_number_total             8346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8se00623g2.cif
_cod_data_source_block           l
_cod_original_formula_sum        'C22.50 H28 K0.50 N6 Ni0.50 O3'
_cod_database_code               1554613
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.912
_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. Others
 Sof(C1SB)=1-FVAR(1)
 Sof(C1SA)=FVAR(1)
3.a Riding coordinates:
 C35(H35A,H35B)
3.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C40(H40A,H40B), C26(H26A,H26B), C32(H32A,H32B), C31(H31A,
 H31B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C38(H38A,H38B),
 C42(H42A,H42B), C33(H33A,H33B), C29(H29A,H29B), C34(H34A,H34B), C36(H36A,H36B),
  C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N9(H9A), C1(H1), N7(H7), C4(H4A), C2(H2A), C9(H9), C10(H10),
 C3(H3), C11(H11), C21(H21), C24(H24), C12(H12), C13(H13), C22(H22), C23(H23),
 C16(H16), C14(H14), C15(H15)
;
_shelx_res_checksum              48076
_shelx_hkl_checksum              50126
_olex2_submission_special_instructions 'No special instructions were received'