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_7132538
_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, C37 H30 N3 P2, 0.5(C6 H4 F2), 0.5(C6 H3 F2)'
_chemical_formula_sum            'C43 H33.5 Cl4 F2 Ga N3 P2'
_chemical_formula_weight         903.743
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_Int_Tables_number      7
_audit_creation_date             2023-11-02
_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                 102.701(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1657(9)
_cell_length_b                   18.5693(11)
_cell_length_c                   19.1345(13)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      2.19
_cell_volume                     4216.9(5)
_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 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_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  0.1165
_diffrn_reflns_av_unetI/netI     0.1345
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68259
_diffrn_reflns_point_group_measured_fraction_full 0.9979
_diffrn_reflns_point_group_measured_fraction_max 0.9979
_diffrn_reflns_theta_full        24.9983
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.10
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1843.231
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.0381
_refine_diff_density_min         -0.7061
_refine_diff_density_rms         0.1448
_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   0.012(9)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             18.5693
_refine_ls_goodness_of_fit_ref   1.0654
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    134
_refine_ls_number_parameters     940
_refine_ls_number_reflns         14851
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0654
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+3.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.996
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              22
_reflns_limit_l_min              -22
_reflns_number_gt                9121
_reflns_number_total             14851
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc05728c2.cif
_cod_data_source_block           2_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7132534--7132538.cif.'
_cod_original_sg_symbol_Hall     ' P -2yac'
_cod_database_code               7132538
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: F15(0.5) F17(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C20(H20), C27(H27), C30(H30), C31(H31), C34(H34), C36(H36),
 C40(H40), C42(H42), C43(H43), C44(H44), C48(H48), C51(H51), C53(H53), C56(H56),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C69(H69),
 C71(H71), C72(H72), C73(H73), C76(H76), C83(H83), C88(H88), C94(H94), C99(H99),
  C16(H16), C22(H22), C28(H28), C29(H29), C38(H38), C39(H39), C45(H45),
 C46(H46), C47(H47), C49(H49), C50(H50), C52(H52), C54(H54), C55(H55), C58(H58),
  C67(H67), C70(H70), C74(H74), C77(H77), C78(H78), C81(H81), C82(H82),
 C87(H87), C90(H90), C95(H95), C97(H97), C120(H120), C129(H129), C134(H134),
 C1(H1), C8(H8), C5(H5), C7(H7), C12(H12), C11(H11), C2(H2), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'