Addition and NN bond cleavage of diazo-compounds by phosphino-phosphenium cations.
Kim, Hyehwang; Lough, Alan; Qu, Zheng-Wang; Grimme, Stefan; Stephan, Douglas W.; Chemical communications (Cambridge, England) 60 (2024) 1031–1034; doi:10.1039/d3cc05728c

data_7132536
_publ_section_title
;
 Addition and N&#xe001;N bond cleavage of diazo-compounds by
 phosphino-phosphenium cations.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1031
_journal_page_last               1034
_journal_paper_doi               10.1039/d3cc05728c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C36 H31 N2 P2, Cl4 Ga, C4 H10 O, 1[C4H10O1]'
_chemical_formula_sum            'C44 H51 Cl4 Ga N2 O2 P2'
_chemical_formula_weight         913.388
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-19 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                95.445(6)
_cell_angle_beta                 108.409(5)
_cell_angle_gamma                91.577(6)
_cell_formula_units_Z            2
_cell_length_a                   11.2788(10)
_cell_length_b                   13.1565(12)
_cell_length_c                   16.1265(15)
_cell_measurement_reflns_used    6319
_cell_measurement_temperature    149.98
_cell_measurement_theta_max      24.02
_cell_measurement_theta_min      2.16
_cell_volume                     2256.1(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 (Bruker AXS, 2021)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      149.98
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_unetI/netI     0.1344
_diffrn_reflns_Laue_measured_fraction_full 0.9974
_diffrn_reflns_Laue_measured_fraction_max 0.9974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42207
_diffrn_reflns_point_group_measured_fraction_full 0.9974
_diffrn_reflns_point_group_measured_fraction_max 0.9974
_diffrn_reflns_theta_full        24.9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.34
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             950.583
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.0736
_refine_diff_density_min         -1.1363
_refine_diff_density_rms         0.1948
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             15.2097
_refine_ls_goodness_of_fit_ref   1.0831
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    75
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0831
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^+8.3622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5225
_reflns_number_total             7940
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc05728c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7132534--7132538.cif.'
_cod_original_formula_sum        'C44 H51 Cl4 Ga1 N2 O2 P2'
_cod_database_code               7132536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31),
  C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40),
 C42(H42), C43(H43), C44(H44), C47(H47), C7(H7), C8(H8), N1(H1), C1(H1a)
2.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C5(H5a,H5b,H5c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 86 electrons were 
found in a volume of 422\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H10O1] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'