Tetramate derivatives by chemoselective Dieckmann ring closure of <i>allo</i>-phenylserines, and their antibacterial activity.
Saney, Liban; Christensen, Kirsten E.; Genov, Miroslav; Pretsch, Alexander; Pretsch, Dagmar; Moloney, Mark G.; Organic & biomolecular chemistry 21 (2023) 4061–4071; doi:10.1039/d3ob00376k

data_7159299
_publ_section_title
;
 Tetramate derivatives by chemoselective Dieckmann ring closure of
 <i>allo</i>-phenylserines, and their antibacterial activity.
;
_journal_issue                   19
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4061
_journal_page_last               4071
_journal_paper_doi               10.1039/d3ob00376k
_journal_volume                  21
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H33 N O6 Si'
_chemical_formula_sum            'C27 H33 N O6 Si'
_chemical_formula_weight         495.65
_chemical_melting_point          ?
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_block_doi                 10.5517/ccdc.csd.cc2bhq5r
_audit_creation_date             2020-02-18
_audit_creation_method           'CRYSTALS_ver_14.61_build_7453 '
_audit_update_record
;
2022-03-18 deposited with the CCDC.	2023-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2357(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.47270(10)
_cell_length_b                   8.76000(10)
_cell_length_c                   28.8275(3)
_cell_measurement_reflns_used    16952
_cell_measurement_temperature    150
_cell_measurement_theta_max      77.02
_cell_measurement_theta_min      3.07
_cell_volume                     2637.44(5)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_av_unetI/netI     0.043
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26682
_diffrn_reflns_theta_full        75.641
_diffrn_reflns_theta_max         77.185
_diffrn_reflns_theta_min         1.537
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.125
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.21
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 4119 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.003(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10665
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.0019599
_refine_ls_shift/su_mean         0.0001134
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0832
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0832
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              10
_reflns_limit_k_min              -11
_reflns_limit_l_max              36
_reflns_limit_l_min              0
_reflns_number_gt                10308
_reflns_number_total             10665
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.23
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0320
_oxford_refine_ls_scale          4.39(4)
_oxford_reflns_number_all        10665
_oxford_structure_analysis_title 7272
_cod_data_source_file            d3ob00376k2.cif
_cod_data_source_block           10-177
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7159291--7159301.cif.
;
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               7159299
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0320
_oxford_refine_ls_wr_factor_all  0.0832
_oxford_hooft_y                  -0.005(8)
_oxford_bijvoet_difference       0.003(7)
_oxford_refined_flack_x          -0.001(12)