(1<i>R</i>,2<i>R</i>)-1,3-Bis(<i>tert</i>-butyldimethylsilyloxy)-2-(4-hydroxybutanamido)-1-(4-nitrophenyl)propane
Johansson, Dorte; Larsen, Frank B.; Bond, Andrew D.; Nielsen, Poul; Acta Crystallographica Section E 60 (2004) o907–o908; doi:10.1107/S1600536804009870

data_2203630
_publ_section_title
(1<i>R</i>,2<i>R</i>)-1,3-Bis(<i>tert</i>-butyldimethylsilyloxy)-2-(4-hydroxybutanamido)-1-(4-nitrophenyl)propane
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o907
_journal_page_last               o908
_journal_paper_doi               10.1107/S1600536804009870
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C25 H46 N2 O6 Si2'
_chemical_formula_moiety         'C25 H46 N2 O6 Si2'
_chemical_formula_sum            'C25 H46 N2 O6 Si2'
_chemical_formula_weight         526.82
_chemical_melting_point          .359E-305
_chemical_name_systematic
;
(1R,2R)-1,3-Bis(tert-butyldimethylsilyloxy)-2-(4-hydroxybutanamido)-
1-(4-nitrophenyl)propane
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.288(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9014(12)
_cell_length_b                   12.0241(10)
_cell_length_c                   17.2103(14)
_cell_measurement_reflns_used    2489
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      18.43
_cell_measurement_theta_min      2.37
_cell_volume                     3082.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'Thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12674
_diffrn_reflns_theta_full        22.02
_diffrn_reflns_theta_max         22.02
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.361
_refine_ls_abs_structure_details
'Friedel opposites (1809 pairs) merged prior to final refinement'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         3985
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0794P)^2^+0.6178P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                2691
_reflns_number_total             3985
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6210.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2203630
_cod_database_fobs_code          2203630