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_7720421
_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_moiety         'C97 H75 Ga N2, 0.625(C4 H10 O2)'
_chemical_formula_sum            'C99.5 H81.25 Ga N2 O1.25'
_chemical_formula_weight         1394.63
_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                90.675(15)
_cell_angle_beta                 102.827(14)
_cell_angle_gamma                97.442(7)
_cell_formula_units_Z            2
_cell_length_a                   13.327(4)
_cell_length_b                   13.562(4)
_cell_length_c                   21.365(10)
_cell_measurement_reflns_used    2694
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.30
_cell_measurement_theta_min      2.40
_cell_volume                     3730(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.2134
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33442
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         1.769
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.4984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.666
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         20973
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.2146
_refine_ls_R_factor_gt           0.0813
_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^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9062
_reflns_number_total             20973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02466h2.cif
_cod_data_source_block           ga01
_cod_original_formula_sum        'C99.50 H81.25 Ga N2 O1.25'
_cod_database_code               7720421
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              65534