Amidine/Amidinate Cobalt Complexes: One-Pot Synthesis, Mechanism, and Photocatalytic Application for Hydrogen Production
Rajak, Sanil; Chair,Khaoula; Rana, Love Karan; Kaur, Prabhjyot; Maris, Thierry; Duong, Adam; Inorganic Chemistry 59 (2020) 14910–14919; doi:10.1021/acs.inorgchem.0c01495

data_4350785
_publ_section_title
;
 Amidine/Amidinate Cobalt Complexes: One-Pot Synthesis, Mechanism, and
 Photocatalytic Application for Hydrogen Production
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14910
_journal_page_last               14919
_journal_paper_doi               10.1021/acs.inorgchem.0c01495
_journal_volume                  59
_journal_year                    2020
_chemical_formula_moiety
'2(C30 H25 Co N14), 4(Cl O4), 4(C4 H8 O2), C7 H5 N'
_chemical_formula_sum            'C83 H87 Cl4 Co2 N29 O24'
_chemical_formula_weight         2134.47
_chemical_name_systematic
;
N'-[4-amino-6-(pyridin-2-yl)-1,3,5-triazin-2-yl]benzenecarboximidamide)
-(N-[4-amino-6-(pyridin-2-yl)-1,3,5-triazin-2-yl]benzenecarboximidamido)-cobalt 
diperchlorate benzonitrile ethyl acetate solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.1400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5415(3)
_cell_length_b                   16.9560(4)
_cell_length_c                   23.1839(6)
_cell_measurement_reflns_used    9528
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.673
_cell_measurement_theta_min      2.845
_cell_volume                     4759.0(2)
_computing_cell_refinement
;
SAINT (2013) V8.37A; Integration Software for Single Crystal Data. 
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT (2013) V8.37A; Integration Software for Single Crystal Data. 
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67565
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.749
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.092
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1164 before and 0.0542 after correction. 
The Ratio of minimum to maximum transmission is 0.7228. 
The \l/2 correction factor is Not present.'
;
_exptl_crystal_colour            'clear light Orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2204
_exptl_crystal_recrystallization_method 'crystallised from AcOEt/Cyanobenzene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0054(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         10955
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+4.0035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10228
_reflns_number_total             10955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4350785.cif
_cod_data_source_block           4350785
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

data item '_exptl_crystal_colour_primary' value 'Orange' was changed
to 'orange' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 

 The Wrong Structure and associated hkl file was deposited. Replaced
 with the correct structure as published ...
;
_cod_database_code               4350785
_cod_database_fobs_code 4350785