Stannyl phosphaketene as a synthon for phosphorus analogues of β-lactam
Luo, Yong-An; Zhao, Zhao; Chen, Ting; Li, Yanguo; Zhao, Yufen; Stephan, Douglas W.; Wu, Yile; Chemical Communications  (2023) –; doi:10.1039/D3CC03117A

data_7132024
_publ_section_title
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 Stannyl phosphaketene as a synthon for phosphorus analogues of \b-lactam
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03117A
_journal_year                    2023
_chemical_formula_moiety         'C25 H7 B F15 O5 P Sn, C7 H8'
_chemical_formula_sum            'C32 H15 B F15 O5 P Sn'
_chemical_formula_weight         924.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-17 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                99.900(3)
_cell_angle_beta                 114.828(2)
_cell_angle_gamma                103.138(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5863(5)
_cell_length_b                   12.5598(6)
_cell_length_c                   13.4404(6)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.428
_cell_measurement_theta_min      3.792
_cell_volume                     1647.63(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61002
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.455
_diffrn_reflns_theta_min         3.791
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.817
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0775 after correction.
The Ratio of minimum to maximum transmission is 0.7743.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.6232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5637
_reflns_number_total             6035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03117a2.cif
_cod_data_source_block           12345
_cod_original_cell_volume        1647.63(13)
_cod_database_code               7132024
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00W(H00W)
2.b Aromatic/amide H refined with riding coordinates:
 C013(H013), C019(H019), C01B(H01G), C01G(H01H), C01I(H01I)
2.c Idealised Me refined as rotating group:
 C015(H01A,H01B,H01C), C01D(H01D,H01E,H01F), C01J(H01J,H01K,H01L)
;
_shelx_res_checksum              21498
_shelx_hkl_checksum              48310
_olex2_submission_special_instructions 'No special instructions were received'