Reactivity of an arsanyl-phosphagallene: decarbonylation of CO2 and COS to form phosphaketenes
Szych, Lilian S.; Bresien, Jonas; Fischer, Lukas; Ernst, Moritz J.; Goicoechea, Jose M.; Chemical Science 16 (2025) 7397–7410; doi:10.1039/D5SC00295H

data_1574164
_publ_section_title
;
 Reactivity of an arsanyl-phosphagallene: decarbonylation of CO2 and COS
 to form phosphaketenes
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              7397
_journal_page_last               7410
_journal_paper_doi               10.1039/D5SC00295H
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C68 H101 As Ga N6 P, C6 H6'
_chemical_formula_sum            'C74 H107 As Ga N6 P'
_chemical_formula_weight         1256.26
_chemical_name_systematic
;
 [{N(2,6-iPr-C6H3)}2(CMe)2CH]Ga[CyNCNCy]PAs[{N(2,6-iPr-C6H3)}2(CH2)2]*C6H6
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2024-12-12 deposited with the CCDC.	2025-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4475(2)
_cell_length_b                   20.8956(3)
_cell_length_c                   24.4457(3)
_cell_measurement_reflns_used    18734
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.3880
_cell_measurement_theta_min      3.6970
_cell_volume                     6869.08(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27676
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.437
_diffrn_reflns_theta_min         3.616
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 5089 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         13450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.1986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                12705
_reflns_number_total             13450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00295h3.cif
_cod_data_source_block           LS056
_cod_depositor_comments
'Adding full bibliography for 1574160--1574169.cif.'
_cod_database_code               1574164
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              2794