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_7132025
_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 H47 B F15 N2 O P Sn'
_chemical_formula_sum            'C56 H47 B F15 N2 O P Sn'
_chemical_formula_weight         1209.42
_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             2023-07-19
_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                84.280(2)
_cell_angle_beta                 75.467(2)
_cell_angle_gamma                86.6760(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4575(3)
_cell_length_b                   15.5646(4)
_cell_length_c                   16.0433(5)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      70.07
_cell_measurement_theta_min      2.85
_cell_volume                     2754.08(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67812
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.170
_diffrn_reflns_theta_min         2.855
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.772
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         10422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.9756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9382
_reflns_number_total             10422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03117a2.cif
_cod_data_source_block           7
_cod_database_code               7132025
_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), C012(H012), C015(H015), C01N(H01N), C020(H020)
2.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C019(H019), C01B(H01B), C01F(H01F), C01G(H01G), C01I(H01I),
 C01M(H01M), C01O(H01O), C01R(H01R), C01U(H01U), C01W(H01W), C01Y(H01Y)
2.c Idealised Me refined as rotating group:
 C00U(H00A,H00B,H00C), C00Z(H00D,H00E,H00F), C01P(H01A,H01C,H01D), C01V(H01E,
 H01H,H01J), C01X(H01K,H01L,H01P), C022(H02A,H02B,H02C), C023(H02D,H02E,H02F),
 C024(H02G,H02H,H02I), C025(H02J,H02K,H02L), C026(H02M,H02N,H02O)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86929
_shelx_hkl_checksum              60028
_shelx_fab_checksum              7146
_olex2_submission_special_instructions 'No special instructions were received'