Synthesis and reactivity of a six-membered heterocyclic 1,3-diphosphaallene.
Sharma, Mahendra K.; Wölper, Christoph; Siera, Hannah; Haberhauer, Gebhard; Schulz, Stephan; Chemical science 16 (2025) 1189–1196; doi:10.1039/d4sc06371f

data_1573371
_publ_section_title
;
 Synthesis and reactivity of a six-membered heterocyclic
 1,3-diphosphaallene.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1189
_journal_page_last               1196
_journal_paper_doi               10.1039/d4sc06371f
_journal_volume                  16
_journal_year                    2025
_chemical_formula_sum            'C79 H111 Ga2 N6 O P2'
_chemical_formula_weight         1362.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9543(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7310(4)
_cell_length_b                   18.2400(4)
_cell_length_c                   39.5206(7)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      80.76
_cell_measurement_theta_min      3.23
_cell_volume                     14863.4(5)
_computing_cell_refinement       'Bruker APEX3(v2017.3-0)'
_computing_data_collection       'Bruker APEX3(v2017.3-0)'
_computing_data_reduction        'Bruker APEX3(v2017.3-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Bruker APEX3(v2017.3-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture (Photon II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/Queen'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0076
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            473924
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         81.015
_diffrn_reflns_theta_min         2.248
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       tablet
_exptl_crystal_F_000             5816
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.771
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         16343
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+31.4654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16272
_reflns_number_total             16343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06371f2.cif
_cod_data_source_block           mks_022m
_cod_depositor_comments
'Adding full bibliography for 1573368--1573371.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1573371
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              24174
_shelx_hkl_checksum              44585