Backbone Deprotonation Defines a Hidden Decomposition Pathway of Diphosphine Ligands
Taylor, Logan; Dilinaer, A. Dina; Boyle, Paul D.; Drover, Marcus W.; Chemical Communications  (2026) –; doi:10.1039/D6CC01011C

data_7135624
_publ_section_title
;
 Backbone deprotonation defines a hidden decomposition pathway of
 diphosphine ligands.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7524
_journal_page_last               7528
_journal_paper_doi               10.1039/d6cc01011c
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C54 H110 Fe2 P6, 2(C24 H20 B)'
_chemical_formula_sum            'C102 H150 B2 Fe2 P6'
_chemical_formula_weight         1695.35
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2026-02-01
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;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-02 deposited with the CCDC.	2026-03-12 downloaded from the CCDC.
;
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
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_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            205319
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.927
_diffrn_reflns_theta_min         2.849
_exptl_absorpt_coefficient_mu    3.703
_exptl_absorpt_correction_T_max  1.000
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.118a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
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_refine_ls_number_reflns         10077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0409
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+8.3343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                9765
_reflns_number_total             10077
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7135623--7135624.cif.'
_cod_original_cell_volume        9574.94(10)
_cod_database_code               7135624
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.837
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C15(H15A,H15B), C25(H25A,H25B), C22(H22A,H22B),
 C19(H19A,H19B), C26(H26A,H26B), C2(H2A,H2B), C23(H23A,H23B), C16(H16A,H16B),
 C6(H6A,H6B), C14(H14A,H14B), C17(H17A,H17B), C3(H3A,H3B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C12(H12), C11(H11), C10(H10), C9(H9), C47(H47), C29(H29), C35(H35),
 C33(H33), C32(H32), C31(H31), C38(H38), C50(H50), C49(H49), C51(H51), C30(H30),
  C36(H36), C48(H48), C37(H37), C45(H45), C41(H41), C44(H44), C43(H43), C42(H42)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C18(H18A,H18B,
 H18C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              52871
_olex2_submission_special_instructions 'No special instructions were received'