Design of a [FeFe] macrocyclic metallotecton for light-driven hydrogen evolution reaction
Rajak, Sanil; Schott, Olivier; Kaur, Prabhjyot; Maris, Thierry; Hanan, Garry S.; Duong, Adam; International Journal Of Hydrogen Energy 45 (2020) 2699–2708; doi:10.1016/j.ijhydene.2019.11.141

data_1559904
_publ_section_title
;
 Design of a [FeFe] macrocyclic metallotecton for light-driven hydrogen
 evolution reaction
;
_journal_name_full               'International Journal Of Hydrogen Energy'
_journal_page_first              2699
_journal_page_last               2708
_journal_paper_doi               10.1016/j.ijhydene.2019.11.141
_journal_volume                  45
_journal_year                    2020
_chemical_formula_moiety
'C33 H37 Fe2 N24 O5 P2, 2(N O3), 3.25(C H4 O)'
_chemical_formula_sum            'C36.25 H50 Fe2 N26 O14.25 P2'
_chemical_formula_weight         1251.66
_chemical_name_systematic
;
(\m-dihydrogen phosphinato)-(\m-methyl phosphito)-tetrakis(6-(2-pyridyl)
-1,3,5-triazine-2,4-diamine)-di-iron dinitrate methanol solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.687(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6206(3)
_cell_length_b                   14.3962(4)
_cell_length_c                   19.5412(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    150
_cell_measurement_theta_max      60.637
_cell_measurement_theta_min      3.339
_cell_volume                     2935.95(15)
_computing_cell_refinement
;
SAINT (2013) V8.38A; 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) V8.38A; 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  'XL (Sheldrick, 2008)'
_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 0.999
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            62514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.704
_diffrn_reflns_theta_min         3.338
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    3.524
_exptl_absorpt_correction_T_max  0.4613
_exptl_absorpt_correction_T_min  0.3269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1236 before and 0.0660 after correction. 
The Ratio of minimum to maximum transmission is 0.7086. 
The \l/2 correction factor is Not present.'
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1291
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0055(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6753
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+1.9273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6096
_reflns_number_total             6753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rm262.cif
_cod_data_source_block           rm262
_cod_database_code               1559904