Electrocatalytic hydrogen production by CN– substituted cobalt triaryl corroles
Liu, Zheng-Yan; Lai, Jia-Wei; Yang, Gang; Ren, Bao-Ping; Lv, Zhou-Yan; Si, Li-Ping; Zhang, Hao; Liu, Hai-Yang; Catalysis Science & Technology 12 (2022) 5125–5135; doi:10.1039/D2CY00606E

data_1567160
_publ_section_title
;
 Electrocatalytic hydrogen production by CN-- substituted cobalt triaryl
 corroles
;
_journal_issue                   16
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5125
_journal_page_last               5135
_journal_paper_doi               10.1039/D2CY00606E
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C57 H36 Co N6 P'
_chemical_formula_sum            'C57 H36 Co N6 P'
_chemical_formula_weight         894.82
_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   geom
_audit_creation_date             2021-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-15 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                91.265(2)
_cell_angle_beta                 108.634(2)
_cell_angle_gamma                94.679(2)
_cell_formula_units_Z            4
_cell_length_a                   14.3899(7)
_cell_length_b                   16.2551(8)
_cell_length_c                   19.6213(9)
_cell_measurement_reflns_used    6004
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.209
_cell_measurement_theta_min      2.193
_cell_volume                     4328.9(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.1133
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45199
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1123 before and 0.0688 after correction. The Ratio of minimum to maximum transmission is 0.8335. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
TITL lzy_0m_a.res in P-1
CELL   14.3899   16.2551   19.6213     91.26    108.63     94.68
SPGR P-1
Q101 0.331 0.301 0.214 !       4.58 eA-3
Q102 0.221 0.419 0.264 !       4.33 eA-3
Q103 0.137 0.512 0.081 !       2.20 eA-3
Q104 0.076 0.452 0.061 !       2.16 eA-3
Q105 0.222 0.338 0.199 !       1.79 eA-3
Q106 0.408 0.444 0.488 !       1.76 eA-3
Q107 0.046 0.583 0.144 !       1.71 eA-3
Q108 0.989 0.510 0.141 !       1.35 eA-3
Q109 0.229 0.524 0.222 !       1.26 eA-3
Q110 0.326 0.327 0.449 !       1.22 eA-3
Q111 0.248 0.363 0.394 !       1.22 eA-3
Q112 0.075 0.523 0.127 !       1.17 eA-3
C113 0.255 0.304 0.156 !       1.10 eA-3
Q114 0.311 0.402 0.434 !       1.09 eA-3
Q115 0.109 0.407 0.184 !       1.06 eA-3
Q116 0.345 0.580 0.167 !       1.04 eA-3
Q117 0.434 0.532 0.171 !       1.03 eA-3
Q118 0.388 0.285 0.426 !       1.03 eA-3
Q119 0.747 0.735 0.311 !       1.01 eA-3
Q120 0.016 0.261 0.031 !       0.99 eA-3
Q121 0.234 0.109 0.111 !       0.99 eA-3
Q122 0.293 0.317 0.389 !       0.96 eA-3
Q123 0.986 0.450 0.118 !       0.93 eA-3
C124 0.269 0.289 0.184 !       0.93 eA-3
Q125 0.953 0.253-0.006 !       0.92 eA-3
Q126 0.706 0.673 0.320 !       0.92 eA-3
Q127 0.138 0.550 0.170 !       0.91 eA-3
Q128 0.043 0.523 0.303 !       0.89 eA-3
Q129 0.815 0.654 0.187 !       0.89 eA-3
Q130 0.312 0.424 0.480 !       0.89 eA-3
Q131 0.683 0.981 0.307 !       0.88 eA-3
Q132 0.610 0.682 0.310 !       0.88 eA-3
Q133 0.033 0.251 0.301 !       0.85 eA-3
Q134 0.372 0.857 0.428 !       0.85 eA-3
Q135 0.423 0.303 0.137 !       0.85 eA-3
Q136 0.825 0.173 0.234 !       0.85 eA-3
Q137 0.970 0.240 0.058 !       0.84 eA-3
Q138 0.110 0.972 0.253 !       0.84 eA-3
Q139 0.488 0.422 0.471 !       0.84 eA-3
Q140 0.172 0.560 0.159 !       0.83 eA-3
Q141 0.268 0.047 0.495 !       0.82 eA-3
Q142 0.045 0.686 0.042 !       0.81 eA-3
Q143 0.518 0.975 0.419 !       0.79 eA-3
Q144 0.026 0.950 0.467 !       0.79 eA-3
Q145 0.893 0.800 0.216 !       0.79 eA-3
Q146 0.957 0.670 0.315 !       0.78 eA-3
Q147 0.122 0.873 0.340 !       0.78 eA-3
Q148 0.862 0.763 0.406 !       0.77 eA-3
Q149 0.567 0.147 0.032 !       0.77 eA-3
Q150 0.453 0.952 0.108 !       0.76 eA-3
Q151 0.719 0.305-0.003 !       0.76 eA-3
Q152 0.029 0.721 0.058 !       0.75 eA-3
Q153 0.363 0.737 0.081 !       0.75 eA-3
Q154 0.481 0.273 0.016 !       0.75 eA-3
Q155 0.498 0.744 0.485 !       0.75 eA-3
Q156 0.930 0.930 0.243 !       0.75 eA-3
Q157 0.935 0.376 0.224 !       0.74 eA-3
Q158 0.247 0.453 0.220 !       0.74 eA-3
Q159 0.652 0.053 0.393 !       0.74 eA-3
Q160 0.513 0.633 0.392 !       0.74 eA-3
Q161 0.793 0.445 0.435 !       0.74 eA-3
Q162 0.359 1.002 0.358 !       0.73 eA-3
Q163 0.083 0.485 0.168 !       0.72 eA-3
Q164 0.931 0.925 0.108 !       0.72 eA-3
Q165 0.278 0.141 0.428 !       0.72 eA-3
Q166 0.061 1.003 0.042 !       0.72 eA-3
Q167 0.594 0.064 0.215 !       0.72 eA-3
Q168 0.263 0.249 0.165 !       0.72 eA-3
Q169 0.253 0.658 0.466 !       0.72 eA-3
Q170 0.970 0.014 0.204 !       0.72 eA-3
Q171 0.731 0.112-0.005 !       0.72 eA-3
Q172 0.062 0.127 0.452 !       0.72 eA-3
Q173 0.793 0.892 0.283 !       0.72 eA-3
Q174 0.579 0.047 0.071 !       0.71 eA-3
Q175 0.497 0.329 0.438 !       0.71 eA-3
Q176 0.568 0.880 0.206 !       0.71 eA-3
Q177 0.345 0.957 0.329 !       0.71 eA-3
Q178 0.485 0.203 0.509 !       0.71 eA-3
Q179 0.529 0.262 0.251 !       0.71 eA-3
Q180 0.339 0.590 0.389 !       0.71 eA-3
Q181 0.314 0.042 0.230 !       0.70 eA-3
Q182 0.589 0.486 0.242 !       0.69 eA-3
Q183 0.544 0.580 0.451 !       0.69 eA-3
Q184 0.999 0.447 0.390 !       0.68 eA-3
Q185 0.969 0.666 0.348 !       0.68 eA-3
Q186 0.856 0.621 0.174 !       0.68 eA-3
Q187 0.191 0.495 0.051 !       0.68 eA-3
Q188 0.201 0.359-0.003 !       0.67 eA-3
Q189 0.858 0.537 0.270 !       0.66 eA-3
Q190 0.105 0.845 0.455 !       0.65 eA-3
Q191 0.073 0.216 0.063 !       0.65 eA-3
Q192 0.938 0.488 0.175 !       0.64 eA-3
Q193 0.595 1.005 0.188 !       0.63 eA-3
Q194 0.389 0.325 0.202 !       0.63 eA-3
Q195 0.891 0.455 0.299 !       0.63 eA-3
Q196 0.112 0.918 0.014 !       0.63 eA-3
Q197 0.761 0.328 0.487 !       0.63 eA-3
Q198 0.671 0.437 0.023 !       0.63 eA-3
Q199 0.425 0.143 0.110 !       0.63 eA-3
;
_refine_diff_density_max         3.210
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         15233
_refine_ls_number_restraints     1687
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+14.0319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9438
_reflns_number_total             15233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy00606e2.cif
_cod_data_source_block           lzy_0m_sq
_cod_depositor_comments
'Adding full bibliography for 1567159--1567160.cif.'
_cod_database_code               1567160
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C03K) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C03C)
\\sim Ueq, Uanis(C03J) \\sim Ueq, Uanis(C035) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.01
Uanis(C03L) \\sim Ueq, Uanis(C03I) \\sim Ueq, Uanis(C03H) \\sim Ueq,
Uanis(C03N) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C0AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C039) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
4. Others
 Fixed Sof: C03K(0.5) H03K(0.5) C4(0.5) H4(0.5) C3(0.5) H3(0.5) C03C(0.5)
 H03C(0.5) C03J(0.5) H03J(0.5) H03A(0.5) H039(0.5) C1(0.35) H1(0.35) C2(0.35)
 H2(0.35) C1AA(0.35) H1AA(0.35) C0AA(0.35) H0AA(0.35) C03H(0.65) H03H(0.65)
 C03I(0.65) H03I(0.65) C03L(0.65) H03L(0.65) C03N(0.65) H03N(0.65) C5AA(0.5)
 H5AA(0.5) C035(0.5) C2AA(0.5) H2AA(0.5) C3AA(0.5) H3AA(0.5) C4AA(0.5)
 H4AA(0.5) C6(0.5) H6(0.5) C6AA(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00P(H00P), C00Q(H00Q), C00R(H00R), C00X(H00X),
 C00Z(H00Z), C011(H011), C014(H014), C016(H016), C018(H018), C01A(H01A),
 C01D(H01D), C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I), C01K(H01K),
 C01M(H01M), C01N(H01N), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T),
 C01U(H01U), C01W(H01W), C020(H020), C023(H023), C024(H024), C027(H027),
 C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02F(H02F),
 C02G(H02G), C02H(H02H), C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M),
 C02N(H02N), C02P(H02P), C02R(H02R), C02S(H02S), C02V(H02V), C02W(H02W),
 C02X(H02X), C02Y(H02Y), C02Z(H02Z), C030(H030), C031(H031), C032(H032),
 C033(H033), C034(H034), C03K(H03K), C4(H4), C3(H3), C03C(H03C), C03J(H03J),
 C036(H036), C038(H038), C039(H03A), C039(H039), C1(H1), C2(H2), C1AA(H1AA),
 C0AA(H0AA), C03A(H03B), C03D(H03D), C03F(H03F), C03G(H03G), C03H(H03H),
 C03I(H03I), C03L(H03L), C03N(H03N), C5AA(H5AA), C2AA(H2AA), C3AA(H3AA),
 C4AA(H4AA), C6(H6)
5.b Fitted hexagon refined as free rotating group:
 C039(C1,C2,C037,C1AA,C0AA), C5AA(C035,C2AA,C3AA,C4AA,C6)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'