Poly-amido-saccharides: Synthesis via Anionic Polymerization of a β-Lactam Sugar Monomer
Eric L. Dane; Mark W. Grinstaff; Journal of the American Chemical Society 134 (2012) 16255–16264; doi:10.1021/ja305900r

data_4118709
_publ_section_title
;
 Poly-amido-saccharides: Synthesis via Anionic Polymerization of a
 \b-Lactam Sugar Monomer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16255
_journal_page_last               16264
_journal_paper_doi               10.1021/ja305900r
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H53 N O5 Si3'
_chemical_formula_sum            'C25 H53 N O5 Si3'
_chemical_formula_weight         531.95
_space_group_IT_number           4
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-12-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.225(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1630(10)
_cell_length_b                   8.5438(7)
_cell_length_c                   16.1345(13)
_cell_measurement_reflns_used    9743
_cell_measurement_temperature    94(2)
_cell_measurement_theta_max      66.100
_cell_measurement_theta_min      4.400
_cell_volume                     1672.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'OLEX2 (Dolmanov, et al. 2009)'
_computing_publication_material  'PublCIF v.1.9.5_c (IUCr)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      94(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Proteum-R'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1405
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44515
_diffrn_reflns_theta_full        66.52
_diffrn_reflns_theta_max         66.52
_diffrn_reflns_theta_min         3.64
_diffrn_standards_decay_%        75
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       needle
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1375P)^2^+1.1179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                4821
_reflns_number_total             5815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305900r_si_002.cif
_cod_data_source_block           dane1a_0m
_cod_database_code               4118709