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_7716946
_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 H28 Cl N6 O2 Zn, C H4 O, Cl'
_chemical_formula_sum            'C27 H32 Cl2 N6 O3 Zn'
_chemical_formula_weight         624.85
_chemical_name_common            ZnBAME
_chemical_name_systematic
'[Zinc (II) N,N?- bis(4-antipyrlmethylidene)ethylenediamine chloride] chloride'
_chemical_properties_physical    Efflorescent,Light-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6505(13)
_cell_length_b                   15.7096(13)
_cell_length_c                   21.6693(18)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.24
_cell_volume                     5668.1(8)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX4 (Bruker AXS, 2018)'
_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 0.965
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 3'
_diffrn_measurement_method       '\w and \y'
_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  0.0978
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53811
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         2.243
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_correction_T_min  0.7297
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, Diethyl Ether'
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.162
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.0054(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   1.301
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5300
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0747
_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^)+(0.0820P)^2^+5.7170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4420
_reflns_number_total             5300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01876a2.cif
_cod_data_source_block           WRM007_a
_cod_depositor_comments
'Adding full bibliography for 7716945--7716947.cif.'
_cod_database_code               7716946
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.667
_shelx_estimated_absorpt_t_max   0.842
_shelx_res_checksum              87510
_shelx_hkl_checksum              7865