Mononuclear Fe(III) Schiff base antipyrine complexes for catalytic hydrogen generation.
Cropley, Jessica D.; Mitchell, Amanda C.; Fritsch, Nicole A.; Ho, Marissa; Wells, Timothy D.; Reynolds, Todd M.; Brennessel, William W.; McNamara, William R.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15421–15426; doi:10.1039/d4dt01876a

data_7716947
_publ_section_title
;
 Mononuclear Fe(III) Schiff base antipyrine complexes for catalytic
 hydrogen generation.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15421
_journal_page_last               15426
_journal_paper_doi               10.1039/d4dt01876a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H30 Fe N6 O4, C3.5 H5, 3(N O3)'
_chemical_formula_sum            'C29.5 H35.5 Fe N9 O13'
_chemical_formula_weight         780.02
_chemical_name_common            'FeBAME (NO3)3'
_chemical_name_systematic
'Diaqua Iron (III) N,N?- bis(4-antipyrlmethylidene)ethylenediamine trinitrate'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-06 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                115.034(2)
_cell_angle_beta                 94.913(2)
_cell_angle_gamma                104.992(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8121(5)
_cell_length_b                   14.4735(7)
_cell_length_c                   15.1409(7)
_cell_measurement_reflns_used    9480
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.20
_cell_volume                     1834.57(16)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX5 (Bruker AXS, 2023)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'SHELXLE (Hubschle, 2011)'
_computing_publication_material  'Mercury 2022.2.2 (CCDC, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 3'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_source         Imus
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75172
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.024
_diffrn_reflns_theta_min         2.204
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       needle
_exptl_crystal_F_000             811
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, Toluene'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0500P)^2^+1.3250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6579
_reflns_number_total             7168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01876a2.cif
_cod_data_source_block           mo_wrm012_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7716945--7716947.cif.'
_cod_original_formula_sum        'C29.50 H35.50 Fe N9 O13'
_cod_database_code               7716947
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              90032
_shelx_hkl_checksum              81963
_shelx_fab_checksum              19855