A tetradentate benzannulated P^N^N^P ligand and its Fe(II) complex: synthesis, characterization, and electrocatalytic hydrogen evolution.
Sidhu, Baldeep K.; Kacperkiewicz, Amelia; Braun, Jason D.; Herbert, David E.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17211–17220; doi:10.1039/d5dt02202a

data_7719773
_publ_section_title
;
 A tetradentate benzannulated P^N^N^P ligand and its Fe(II) complex:
 synthesis, characterization, and electrocatalytic hydrogen evolution.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17211
_journal_page_last               17220
_journal_paper_doi               10.1039/d5dt02202a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C52 H38 N2 P2, 1.5[C5H12]'
_chemical_formula_sum            'C52 H38 N2 P2'
_chemical_formula_weight         752.78
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-09-12 deposited with the CCDC.	2025-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                80.538(2)
_cell_angle_beta                 80.003(2)
_cell_angle_gamma                76.315(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3919(6)
_cell_length_b                   14.2984(9)
_cell_length_c                   17.6937(11)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.94
_cell_volume                     2254.6(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Quest ECO CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.074
_diffrn_reflns_theta_min         2.254
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0948 before and 0.0794 after correction.
The Ratio of minimum to maximum transmission is 0.8649.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0557P)^2^+4.5520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7342
_reflns_number_total             9831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02202a2.cif
_cod_data_source_block           deh288
_cod_depositor_comments
'Adding full bibliography for 7719773--7719774.cif.'
_cod_database_code               7719773
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.943
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C29(H29), C30(H30), C31(H31), C32(H32), C37(H37), C39(H39), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
  C52(H52)
2.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C40(H40a,H40b,H40c)
;
_shelx_res_checksum              76610
_shelx_fab_checksum              13142
_olex2_submission_special_instructions 'No special instructions were received'