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_1573368
_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            'C59 H82 Ga2 N4 O P2'
_chemical_formula_weight         1064.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 96.3710(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5423(10)
_cell_length_b                   13.8181(6)
_cell_length_c                   17.4303(8)
_cell_measurement_reflns_used    9463
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      80.19
_cell_measurement_theta_min      3.71
_cell_volume                     5635.2(4)
_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 0.992
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            210810
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.782
_diffrn_reflns_theta_min         3.715
_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    2.023
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         12297
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0301P)^2^+3.1832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12245
_reflns_number_total             12297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06371f2.cif
_cod_data_source_block           mks_018m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1573368--1573371.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1573368
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.697
_shelx_res_checksum              31699
_shelx_hkl_checksum              78521