Gallium phosphaketenes derived from bis(imino)acenaphthenes (bian): synthesis and reactivity towards a trityl radical and bian-gallylene.
Skatova, Alexandra A.; Bazanov, Andrey A.; Baranov, Evgeny V.; Kiskin, Mikhail A.; Ketkov, Sergey Yu; Fedushkin, Igor L.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 2080–2087; doi:10.1039/d5dt02466h

data_7720422
_publ_section_title
;
 Gallium phosphaketenes derived from bis(imino)acenaphthenes (bian):
 synthesis and reactivity towards a trityl radical and bian-gallylene.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2080
_journal_page_last               2087
_journal_paper_doi               10.1039/d5dt02466h
_journal_volume                  55
_journal_year                    2026
_chemical_formula_sum            'C93 H76 Ga N2 O P'
_chemical_formula_weight         1338.24
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-08-10 deposited with the CCDC.	2025-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                68.618(3)
_cell_angle_beta                 86.435(3)
_cell_angle_gamma                83.840(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2228(4)
_cell_length_b                   14.9094(4)
_cell_length_c                   20.3396(6)
_cell_measurement_reflns_used    15088
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9870
_cell_measurement_theta_min      2.1000
_cell_volume                     3430.46(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_structure_refinement  SHELXL-2019/3
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0704
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70217
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       plate
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         12113
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0737
_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^)+(0.0790P)^2^+14.5325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.2167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8529
_reflns_number_total             12113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02466h2.cif
_cod_data_source_block           gabbianpco1
_cod_original_cell_volume        3430.45(19)
_cod_database_code               7720422
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.807
_shelx_estimated_absorpt_t_max   0.954
_oxdiff_exptl_absorpt_empirical_full_min 0.859
_oxdiff_exptl_absorpt_empirical_full_max 1.219
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              86647