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_7132534
_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_absolute_configuration unk
_chemical_formula_moiety         'Cl4 Ga, C36 H30 Cl N2 P2, C H Cl3'
_chemical_formula_sum            'C37 H31 Cl8 Ga N2 P2'
_chemical_formula_weight         918.963
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_Int_Tables_number      29
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.402(4)
_cell_length_b                   11.4012(12)
_cell_length_c                   16.4543(16)
_cell_measurement_reflns_used    3781
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      19.53
_cell_measurement_theta_min      2.22
_cell_volume                     7954.6(14)
_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      150.02
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9999
_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  0.1513
_diffrn_reflns_av_unetI/netI     0.1834
_diffrn_reflns_Laue_measured_fraction_full 0.9999
_diffrn_reflns_Laue_measured_fraction_max 0.9999
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            76114
_diffrn_reflns_point_group_measured_fraction_full 0.9875
_diffrn_reflns_point_group_measured_fraction_max 0.9875
_diffrn_reflns_theta_full        24.9995
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.96
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0718 after correction.
The Ratio of minimum to maximum transmission is 0.7619.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             3726.741
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.3420
_refine_diff_density_min         -0.9420
_refine_diff_density_rms         0.1688
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.002(12)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             21.2010
_refine_ls_goodness_of_fit_ref   0.9821
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    124
_refine_ls_number_parameters     901
_refine_ls_number_reflns         13861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9821
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.974
_reflns_limit_h_max              50
_reflns_limit_h_min              -50
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              -19
_reflns_number_gt                9590
_reflns_number_total             13861
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc05728c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7132534--7132538.cif.'
_cod_original_sg_symbol_Hall     ' P 2c -2ac'
_cod_database_code               7132534
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C34(H34), C39(H39),
 C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C55(H55), C56(H56), C59(H59),
  C60(H60), C61(H61), C62(H62), C66(H66), C68(H68), C73(H73), C75(H75),
 C78(H78), C82(H82), C83(H83), C97(H97), C131(H131), C141(H141), C23(H23),
 C27(H27), C28(H28), C30(H30), C31(H31), C37(H37), C38(H38), C40(H40), C41(H41),
  C44(H44), C47(H47), C50(H50), C51(H51), C53(H53), C57(H57), C58(H58),
 C64(H64), C69(H69), C72(H72), C74(H74), C76(H76), C79(H79), C80(H80), C84(H84),
  C90(H90), C91(H91), C96(H96), C107(H107), C116(H116), C14(H14), C1(H1),
 C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'