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_7132537
_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, C40 H43 N2 O4 P2, C H2 Cl2'
_chemical_formula_sum            'C41 H45 Cl6 Ga N2 O4 P2'
_chemical_formula_weight         974.211
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_Int_Tables_number      1
_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
;
2023-12-12 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                96.899(17)
_cell_angle_beta                 93.763(19)
_cell_angle_gamma                95.349(14)
_cell_formula_units_Z            1
_cell_length_a                   9.792(7)
_cell_length_b                   10.064(7)
_cell_length_c                   12.020(8)
_cell_measurement_reflns_used    324
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      15.34
_cell_measurement_theta_min      2.78
_cell_volume                     1167.3(14)
_computing_cell_refinement       APEX4
_computing_data_collection       'APEX4 (Bruker AXS, 2021)'
_computing_data_reduction        APEX4
_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 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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  0.1140
_diffrn_reflns_av_unetI/netI     0.1294
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 1.0000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49804
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.9995
_diffrn_reflns_theta_full        24.9997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.7121
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0839 before and 0.0742 after correction.
The Ratio of minimum to maximum transmission is 0.8947.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             501.603
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.7068
_refine_diff_density_min         -0.5220
_refine_diff_density_rms         0.0968
_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   0.139(10)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.8966
_refine_ls_goodness_of_fit_ref   1.0272
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     538
_refine_ls_number_reflns         8206
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0272
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.0014
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                6092
_reflns_number_total             8206
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc05728c2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7132534--7132538.cif.'
_cod_original_cell_volume        1167.2(14)
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               7132537
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Ga1(0.85) Cl5(0.85) Cl6(0.85) Ga2(0.15) Cl9(0.15) Cl8(0.15)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24),
 C26(H26), C30(H30), C31(H31), C32(H32), C36(H36), C38(H38), C39(H39), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51),
 C52(H52), C55(H55)
3.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C33(H33a,H33b,H33c), C37(H37a,H37b,H37c), C49(H49a,H49b,
 H49c), C50(H50a,H50b,H50c), C59(H59a,H59b,H59c)
;
_olex2_submission_special_instructions 'No special instructions were received'