Probing the peripheral role of amines in photo- and electrocatalytic H<sub>2</sub> production by molecular cobalt complexes.
Dolui, Dependu; Mir, Ab Qayoom; Dutta, Arnab; Chemical communications (Cambridge, England) 56 (2020) 14841–14844; doi:10.1039/d0cc05786j

data_7127429
_publ_section_title
;
 Probing the peripheral role of amines in photo- and electrocatalytic
 H<sub>2</sub> production by molecular cobalt complexes.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14841
_journal_page_last               14844
_journal_paper_doi               10.1039/d0cc05786j
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H36 Cl2 Co2 N10 O8'
_chemical_formula_sum            'C22 H36 Cl2 Co2 N10 O8'
_chemical_formula_weight         757.37
_chemical_name_systematic        C2
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_Int_Tables_number      170
_audit_creation_date             2020-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-22 deposited with the CCDC.	2020-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   20.3990(12)
_cell_length_b                   20.3990(12)
_cell_length_c                   14.7613(9)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.43
_cell_volume                     5319.5(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.9909
_diffrn_measured_fraction_theta_max 0.9909
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49657
_diffrn_reflns_theta_full        28.4346
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         3.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1000 before and 0.0613 after correction. The Ratio of minimum to maximum transmission is 0.7534. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4184
_exptl_crystal_description       plate
_exptl_crystal_F_000             2346.9173
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.5347
_refine_diff_density_min         -0.2467
_refine_diff_density_rms         0.0687
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.010(8)
_refine_ls_d_res_high            0.7463
_refine_ls_d_res_low             6.0837
_refine_ls_goodness_of_fit_ref   0.9919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8863
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9919
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.989
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                8389
_reflns_number_total             8863
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc05786j2.cif
_cod_data_source_block           ET_AM_AD_2020_0m_a
_cod_original_cell_volume        5319.5(6)
_cod_original_sg_symbol_Hall     ' P 65'
_cod_database_code               7127429
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N6(H6a,H6b), C14(H14a,H14b)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10)
2.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C18(H18a,H18b,H18c), C15(H15a,H15b,H15c), C22(H22a,H22b,
 H22c), C5(H5a,H5b,H5c), C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C4(H4a,H4b,H4c)
;
_olex2_submission_original_sample_id C2_ET_AM_AD_2020
_olex2_submission_special_instructions 'No special instructions were received'