Unexpected bonding ambiguity of the open/closed-shell R<sub>2</sub>PO ligand family: the case of phosphinoyl <i>vs.</i> phosphoryl if bound to transition metals in their low oxidation state.
Brehm, Philipp C.; Schnakenburg, Gregor; Frontera, Antonio; Bill, Eckhard; Schiemann, Olav; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12349–12357; doi:10.1039/d5dt01459j

data_7719362
_publ_section_title
;
 Unexpected bonding ambiguity of the open/closed-shell R<sub>2</sub>PO
 ligand family: the case of phosphinoyl <i>vs.</i> phosphoryl if bound to
 transition metals in their low oxidation state.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12349
_journal_page_last               12357
_journal_paper_doi               10.1039/d5dt01459j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C17 H28 Fe N3 O5 P'
_chemical_formula_sum            'C17 H28 Fe N3 O5 P'
_chemical_formula_weight         441.24
_chemical_name_systematic        PB-142
_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             2019-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2025-01-13 deposited with the CCDC.	2025-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                71.066(6)
_cell_angle_beta                 81.708(6)
_cell_angle_gamma                84.096(6)
_cell_formula_units_Z            2
_cell_length_a                   8.9054(7)
_cell_length_b                   9.8984(8)
_cell_length_c                   12.7846(10)
_cell_measurement_reflns_used    5429
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.59
_cell_volume                     1052.94(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10956
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         2.704
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.8309
_exptl_absorpt_correction_T_min  0.5415
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         10956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0654P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7899
_reflns_number_total             10956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01459j3.cif
_cod_data_source_block           2b
_cod_database_code               7719362
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.886
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5822(10)
 0.4178(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              94939
_shelx_hkl_checksum              71251
_olex2_submission_special_instructions 'No special instructions were received'