A cobalt molecular catalyst for hydrogen evolution reaction with remarkable activity in phosphate buffered water solution
Trotta, Caterina; Dahiya, Pardeep; Baldinelli, Lorenzo; Menendez Rodriguez, Gabriel; Chakraborty, Priyanka; Bistoni, Giovanni; De Angelis, Filippo; Sundararaju, Basker; Macchioni, Alceo; Catalysis Science & Technology 14 (2024) 3699–3706; doi:10.1039/D4CY00209A

data_1571728
_publ_section_title
;
 A cobalt molecular catalyst for hydrogen evolution reaction with
 remarkable activity in phosphate buffered water solution
;
_journal_issue                   13
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3699
_journal_page_last               3706
_journal_paper_doi               10.1039/D4CY00209A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C17 H25 Co I N2, I'
_chemical_formula_sum            'C17 H25 Co I2 N2'
_chemical_formula_weight         570.144
_chemical_name_systematic        Complex-2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                89.106(2)
_cell_angle_beta                 83.431(2)
_cell_angle_gamma                76.170(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2020(7)
_cell_length_b                   9.8816(9)
_cell_length_c                   12.3164(11)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.390
_cell_measurement_theta_min      2.228
_cell_volume                     962.86(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.9983
_diffrn_reflns_Laue_measured_fraction_max 0.9958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15272
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.9958
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1915 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.6720.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       needle
_exptl_crystal_F_000             547.299
_exptl_crystal_preparation       'Slow evaporation'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.8570
_refine_diff_density_min         -1.1378
_refine_diff_density_rms         0.1521
_refine_ls_d_res_high            0.7474
_refine_ls_d_res_low             7.9123
_refine_ls_goodness_of_fit_ref   0.7766
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.7766
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4352
_reflns_number_total             4792
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cy00209a2.cif
_cod_data_source_block           19sepa_1_0m
_cod_depositor_comments
'Adding full bibliography for 1571727--1571728.cif.'
_cod_database_code               1571728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C13(H13), C12(H12)
2.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C17(H17a,H17b,H17c)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id Complex-2
_olex2_submission_special_instructions 'No special instructions were received'