Crystal structure of 1R,5S,8R,9S-8-azidomethyl-2-benzyl-6,6-dimethyl- 3,7-dioxa-2-aza-bicyclo[3.3.1]nonan-9-ol, C~16~H~22~N~4~O~3~
Al-Harrasi, A.; Brüdgam, I.; Hartl, H.; Reißig, H.-U.; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 599–600; doi:

data_8101877
_publ_section_title
;
Crystal structure of 1R,5S,8R,9S-8-azidomethyl-2-benzyl-6,6-dimethyl-
3,7-dioxa-2-aza-bicyclo[3.3.1]nonan-9-ol, C~16~H~22~N~4~O~3~
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              599
_journal_page_last               600
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C16 H22 N4 O3'
_chemical_formula_weight         318.38
_chemical_name_systematic
; 
1R,5S,8R,9S-8-azidomethyl-2-benzyl-6,6-dimethyl-3,7-dioxa-2-aza-
bicyclo[3.3.1]nonan-9-ol
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   5.959(5)
_cell_length_b                   8.099(5)
_cell_length_c                   33.942(5)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.58
_cell_volume                     1638.1(17)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'phi/omega, \D\w = .3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8672
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         2.40
_diffrn_standards_interval_count '20 sec/frame'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_coef       0.0114(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         1690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.831
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                1281
_reflns_number_total             1690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1657.cff
_cod_data_source_block           orgal6m
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               8101877