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_7132026
_publ_section_title
;
 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
'C56 H51 B F15 N2 O5 P Sn, 1.6(C H2 Cl2), C H2 Cl0.5'
_chemical_formula_sum            'C58.6 H56.2 B Cl3.7 F15 N2 O5 P Sn'
_chemical_formula_weight         1445.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-20 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9857(3)
_cell_length_b                   18.8170(4)
_cell_length_c                   24.5153(6)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      2.97
_cell_volume                     6418.5(2)
_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      200.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0959
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            113733
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         3.494
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.624
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             2919
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         11344
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+9.2113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9403
_reflns_number_total             11344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03117a2.cif
_cod_data_source_block           f3
_cod_original_formula_sum        'C58.60 H56.20 B Cl3.70 F15 N2 O5 P Sn'
_cod_database_code               7132026
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C9 \\sim C8-C10
 with sigma of 0.02
 Cl03-C02A \\sim Cl-C02B
 with sigma of 0.02
 Cl00-C02A \\sim Cl6-C02B
 with sigma of 0.02
 Cl03-Cl00 \\sim Cl-Cl6
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C60 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Cl4 \\sim C59 \\sim Cl5: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Cl \\sim C02B \\sim Cl6: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Cl03 \\sim C02A \\sim Cl00: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
4. Others
 Sof(H8BC)=Sof(H8BD)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=1-FVAR(1)
 Sof(H8AA)=Sof(H8AB)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Fixed Sof: Cl03(0.9) Cl00(0.9) C02A(0.9) H02A(0.9) H02B(0.9) Cl4(0.4)
 Cl5(0.4) C59(0.4) H59A(0.4) H59B(0.4) Cl1(0.5) Cl3(0.2) Cl2(0.2) C60(0.2)
 H60A(0.2) H60B(0.2) Cl(0.1) C02B(0.1) H02C(0.1) H02D(0.1) Cl6(0.1)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C23(H23), C35(H35), C26(H26), C38(H38)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8AA,H8AB), C8(H8BC,H8BD), C02A(H02A,H02B), C59(H59A,H59B),
 C58(H58A,H58B), C60(H60A,H60B), C02B(H02C,H02D)
5.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C31(H31), C20(H20), C18(H18), C30(H30), C19(H19)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C36(H36A,H36B,H36C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C37(H37A,
 H37B,H37C), C25(H25A,H25B,H25C), C6(H6A,H6B,H6C), C39(H39A,H39B,H39C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              16007
_shelx_hkl_checksum              53243
_olex2_submission_special_instructions 'No special instructions were received'