 
data_mc92p2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common
;
 Boc-5-amino-2,2,5,5-tetramethyl-pent-3-(E)-enoyl-NHiPr
;
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C17 H32 N2 O3' 
_chemical_formula_weight          312.44

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    5.990(2)
_cell_length_b                    8.937(2)
_cell_length_c                    17.928(3)
_cell_angle_alpha                 88.95(5)
_cell_angle_beta                  87.04(8)
_cell_angle_gamma                 80.67(7)
_cell_volume                      945.7(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     48
_cell_measurement_theta_min       12
_cell_measurement_theta_max       20
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.097          
_exptl_crystal_F_000              344
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.55
_exptl_crystal_size_mid           0.35
_exptl_crystal_size_min           0.10
_exptl_absorpt_coefficient_mu     0.594
_shelx_estimated_absorpt_T_min    0.736
_shelx_estimated_absorpt_T_max    0.943
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_type            CuK\a
_diffrn_source                    'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type   'Philips PW1100 diffractometer'
_diffrn_measurement_method        'θ-2θ scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2793
_diffrn_reflns_av_unetI/netI      0.0078
_diffrn_reflns_av_R_equivalents   0.000
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          4.940
_diffrn_reflns_theta_max          60.001
_diffrn_reflns_theta_full         60.001
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              2793
_reflns_number_gt                 2526
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution   'SIR2002 (Burla et al. 2002)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1352P)²+0.3241P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.026(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2793
_refine_ls_number_parameters      200
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0736
_refine_ls_R_factor_gt            0.0692
_refine_ls_wR_factor_ref          0.2017
_refine_ls_wR_factor_gt           0.1924
_refine_ls_goodness_of_fit_ref    1.059
_refine_ls_restrained_S_all       1.059
_refine_ls_shift/su_max           0.009
_refine_ls_shift/su_mean          0.002
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C01 C 0.0530(4) 0.2348(3) 0.60901(13) 0.0575(6) Uani 1 1 d . . . . .
C02 C -0.1001(5) 0.1220(4) 0.59021(17) 0.0789(9) Uani 1 1 d . . . . .
H02A H -0.0122 0.0225 0.5859 0.118 Uiso 1 1 calc R U . . .
H02B H -0.1685 0.1508 0.5437 0.118 Uiso 1 1 calc R U . . .
H02C H -0.2164 0.1217 0.6291 0.118 Uiso 1 1 calc R U . . .
C03 C 0.2504(6) 0.2277(5) 0.55319(16) 0.0905(10) Uani 1 1 d . . . . .
H03A H 0.3418 0.3019 0.5653 0.136 Uiso 1 1 calc R U . . .
H03B H 0.1956 0.2482 0.5041 0.136 Uiso 1 1 calc R U . . .
H03C H 0.3400 0.1284 0.5545 0.136 Uiso 1 1 calc R U . . .
C04 C -0.0836(5) 0.3907(3) 0.61685(19) 0.0808(9) Uani 1 1 d . . . . .
H04A H -0.2145 0.3862 0.6495 0.121 Uiso 1 1 calc R U . . .
H04B H -0.1309 0.4281 0.5687 0.121 Uiso 1 1 calc R U . . .
H04C H 0.0073 0.4575 0.6374 0.121 Uiso 1 1 calc R U . . .
OU O 0.1296(3) 0.17667(17) 0.68180(8) 0.0574(5) Uani 1 1 d . . . . .
C0 C 0.2616(4) 0.2503(2) 0.72279(12) 0.0463(6) Uani 1 1 d . . . . .
O0 O 0.3454(3) 0.35844(18) 0.70109(9) 0.0582(5) Uani 1 1 d . . . . .
N1 N 0.2811(3) 0.1832(2) 0.79004(10) 0.0490(5) Uani 1 1 d . . . . .
H1 H 0.2094 0.1085 0.7991 0.059 Uiso 1 1 calc R U . . .
C1D C 0.4158(4) 0.2278(2) 0.84945(12) 0.0487(6) Uani 1 1 d . . . . .
C1D1 C 0.6638(5) 0.2113(3) 0.82344(17) 0.0705(8) Uani 1 1 d . . . . .
H1D1 H 0.7196 0.1072 0.8115 0.106 Uiso 1 1 calc R U . . .
H1D2 H 0.7494 0.2426 0.8625 0.106 Uiso 1 1 calc R U . . .
H1D3 H 0.6792 0.2736 0.7799 0.106 Uiso 1 1 calc R U . . .
C1D2 C 0.3887(5) 0.1199(3) 0.91527(14) 0.0642(7) Uani 1 1 d . . . . .
H1D4 H 0.2318 0.1303 0.9316 0.096 Uiso 1 1 calc R U . . .
H1D5 H 0.4755 0.1443 0.9556 0.096 Uiso 1 1 calc R U . . .
H1D6 H 0.4419 0.0174 0.9000 0.096 Uiso 1 1 calc R U . . .
C1G C 0.3393(4) 0.3893(3) 0.87464(13) 0.0575(6) Uani 1 1 d . . . . .
H1G H 0.4332 0.4266 0.9070 0.069 Uiso 1 1 calc R U . . .
C1B C 0.1614(4) 0.4821(3) 0.85732(13) 0.0528(6) Uani 1 1 d . . . . .
H1B H 0.0608 0.4433 0.8281 0.063 Uiso 1 1 calc R U . . .
C1A C 0.0968(4) 0.6474(2) 0.87905(12) 0.0480(6) Uani 1 1 d . . . . .
C1A1 C -0.1586(4) 0.6784(3) 0.89272(16) 0.0650(7) Uani 1 1 d . . . . .
H1A1 H -0.2299 0.6598 0.8478 0.097 Uiso 1 1 calc R U . . .
H1A2 H -0.2051 0.7822 0.9070 0.097 Uiso 1 1 calc R U . . .
H1A3 H -0.2023 0.6129 0.9320 0.097 Uiso 1 1 calc R U . . .
C1A2 C 0.2057(5) 0.6909(3) 0.94919(14) 0.0638(7) Uani 1 1 d . . . . .
H1A4 H 0.1597 0.6325 0.9910 0.096 Uiso 1 1 calc R U . . .
H1A5 H 0.1580 0.7969 0.9587 0.096 Uiso 1 1 calc R U . . .
H1A6 H 0.3676 0.6705 0.9418 0.096 Uiso 1 1 calc R U . . .
C1 C 0.1593(4) 0.7549(2) 0.81569(13) 0.0498(6) Uani 1 1 d . . . . .
O1 O 0.1068(4) 0.89321(18) 0.82361(11) 0.0709(6) Uani 1 1 d . . . . .
NT N 0.2669(3) 0.6942(2) 0.75430(10) 0.0546(6) Uani 1 1 d . . . . .
HT H 0.2946 0.5970 0.7510 0.066 Uiso 1 1 calc R U . . .
CT1 C 0.3408(5) 0.7847(3) 0.69200(13) 0.0591(7) Uani 1 1 d . . . . .
HT1 H 0.2462 0.8850 0.6937 0.071 Uiso 1 1 calc R U . . .
CT2 C 0.3065(6) 0.7115(4) 0.61862(15) 0.0800(9) Uani 1 1 d . . . . .
HT2A H 0.3875 0.6096 0.6177 0.120 Uiso 1 1 calc R U . . .
HT2B H 0.3623 0.7687 0.5779 0.120 Uiso 1 1 calc R U . . .
HT2C H 0.1481 0.7099 0.6138 0.120 Uiso 1 1 calc R U . . .
CT3 C 0.5820(6) 0.8051(4) 0.6983(2) 0.0910(10) Uani 1 1 d . . . . .
HT3A H 0.5974 0.8542 0.7445 0.136 Uiso 1 1 calc R U . . .
HT3B H 0.6260 0.8663 0.6573 0.136 Uiso 1 1 calc R U . . .
HT3C H 0.6775 0.7078 0.6972 0.136 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C01 OU 1.464(3) . ?
C01 C04 1.502(4) . ?
C01 C03 1.503(4) . ?
C01 C02 1.522(4) . ?
OU C0 1.358(3) . ?
C0 O0 1.209(3) . ?
C0 N1 1.338(3) . ?
N1 C1D 1.467(3) . ?
C1D C1G 1.512(3) . ?
C1D C1D1 1.518(4) . ?
C1D C1D2 1.529(3) . ?
C1G C1B 1.287(4) . ?
C1B C1A 1.518(3) . ?
C1A C1A1 1.518(3) . ?
C1A C1A2 1.530(3) . ?
C1A C1 1.544(3) . ?
C1 O1 1.234(3) . ?
C1 NT 1.325(3) . ?
NT CT1 1.459(3) . ?
CT1 CT3 1.496(4) . ?
CT1 CT2 1.518(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
OU C01 C04 110.3(2) . . ?
OU C01 C03 110.5(2) . . ?
C04 C01 C03 113.4(3) . . ?
OU C01 C02 101.0(2) . . ?
C04 C01 C02 109.9(2) . . ?
C03 C01 C02 111.0(3) . . ?
C0 OU C01 121.57(18) . . ?
O0 C0 N1 126.6(2) . . ?
O0 C0 OU 124.8(2) . . ?
N1 C0 OU 108.59(19) . . ?
C0 N1 C1D 124.86(19) . . ?
N1 C1D C1G 113.10(19) . . ?
N1 C1D C1D1 110.37(19) . . ?
C1G C1D C1D1 108.1(2) . . ?
N1 C1D C1D2 106.44(18) . . ?
C1G C1D C1D2 109.18(19) . . ?
C1D1 C1D C1D2 109.6(2) . . ?
C1B C1G C1D 128.6(2) . . ?
C1G C1B C1A 127.5(2) . . ?
C1B C1A C1A1 107.3(2) . . ?
C1B C1A C1A2 114.6(2) . . ?
C1A1 C1A C1A2 108.4(2) . . ?
C1B C1A C1 111.71(18) . . ?
C1A1 C1A C1 107.7(2) . . ?
C1A2 C1A C1 106.88(19) . . ?
O1 C1 NT 122.4(2) . . ?
O1 C1 C1A 119.3(2) . . ?
NT C1 C1A 118.33(18) . . ?
C1 NT CT1 123.06(19) . . ?
NT CT1 CT3 110.9(2) . . ?
NT CT1 CT2 109.9(2) . . ?
CT3 CT1 CT2 111.4(3) . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C04 C01 OU C0 -59.4(3) . . . . ?
C03 C01 OU C0 66.8(3) . . . . ?
C02 C01 OU C0 -175.6(2) . . . . ?
C01 OU C0 O0 -7.7(3) . . . . ?
C01 OU C0 N1 172.15(19) . . . . y
O0 C0 N1 C1D -1.9(4) . . . . ?
OU C0 N1 C1D 178.29(18) . . . . ?
C0 N1 C1D C1G 60.4(3) . . . . y
C0 N1 C1D C1D1 -60.9(3) . . . . ?
C0 N1 C1D C1D2 -179.7(2) . . . . ?
N1 C1D C1G C1B 8.9(4) . . . . y
C1D1 C1D C1G C1B 131.4(3) . . . . ?
C1D2 C1D C1G C1B -109.4(3) . . . . ?
C1D C1G C1B C1A -175.3(2) . . . . y
C1G C1B C1A C1A1 -143.5(3) . . . . ?
C1G C1B C1A C1A2 -23.1(4) . . . . ?
C1G C1B C1A C1 98.7(3) . . . . y
C1B C1A C1 O1 176.4(2) . . . . ?
C1A1 C1A C1 O1 58.8(3) . . . . ?
C1A2 C1A C1 O1 -57.5(3) . . . . ?
C1B C1A C1 NT -3.3(3) . . . . y
C1A1 C1A C1 NT -120.9(2) . . . . ?
C1A2 C1A C1 NT 122.8(2) . . . . ?
O1 C1 NT CT1 2.4(4) . . . . ?
C1A C1 NT CT1 -177.9(2) . . . . y
C1 NT CT1 CT3 94.8(3) . . . . ?
C1 NT CT1 CT2 -141.5(3) . . . . ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
NT HT O0  0.86 2.30 3.120(3) 160.6 .
N1 H1 O1  0.86 2.14 2.988(3) 166.9 1_545
 
_refine_diff_density_max    0.612
_refine_diff_density_min   -0.336
_refine_diff_density_rms    0.064

#===END===