Cobalt, nickel, and iron complexes of 8-hydroxyquinoline-di(2-picolyl)amine for light-driven hydrogen evolution
Carmos dos Santos, Nadia Alessandra; Natali, Mirco; Badetti, Elena; Wurst, Klaus; Licini, Giulia; ZONTA, CRISTIANO; Dalton Transactions  (2017) –; doi:10.1039/C7DT02666H

data_7044651
_publ_section_title
;
 Cobalt, nickel, and iron complexes of
 8-hydroxyquinoline-di(2-picolyl)amine for light-driven hydrogen evolution
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT02666H
_journal_year                    2017
_chemical_formula_sum            'C50 H48 Cl3 Fe2 N11 O15'
_chemical_formula_weight         1261.04
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-14 deposited with the CCDC.
2017-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                86.2019(14)
_cell_angle_beta                 83.5197(14)
_cell_angle_gamma                68.4545(13)
_cell_formula_units_Z            2
_cell_length_a                   12.5578(4)
_cell_length_b                   12.6591(5)
_cell_length_c                   18.4393(6)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.2
_cell_volume                     2708.09(17)
_computing_cell_refinement       'Bruker SAINT-V 8.34A'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT-V 8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL-XT-2014/4 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2014/5)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         9786
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+2.3799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8202
_reflns_number_total             9786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02666h2.cif
_cod_data_source_block           fe
_cod_database_code               7044651
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              98193