#\#CIF_1.1
 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2010-03-29 at 11:53:44
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.4
#  Request file    : c:\wingx\files\archive.reqdat
#  CIF files read  : ele101
 
#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#
 
data_global
 
#------------------ AUDIT DETAILS -------------------------------------------#
 
_audit_creation_date            2010-03-29
_audit_creation_method          'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.4
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record            ?
 
#==============================================================================
#
# SUBMISSION DETAILS
 
_publ_contact_author_name            'Sironi, Angelo'
# Name of author for correspondence
 
_publ_contact_author_address
;Department of Structural Chemistry
University of Milan
Via Venezian 21
Milano, Italy
;
# Address of author for correspondence
 
_publ_contact_author_email           angelo.sironi@unimi.it
_publ_contact_author_fax             '+39 02 50314454'
_publ_contact_author_phone           '+39 02 50314448'
 
_publ_contact_letter
;
 Submission dated :2010-03-29
 
Please consider this CIF for submission to the Cambridge Crystallographic
Data Centre. I certify that all authors have seen and approved of this
submission, that all have made significant scientific contributions to the
work reported, and that all share responsibility and accountability for
the results.
 
This CIF  is submitted as a personal communication
 
This CIF is submitted as part of a journal submission
<Insert Journal details here>
 
;
 
 
#==============================================================================
 
#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#
 
data_ele101
 
_audit_creation_date                    2010-03-29T11:53:44-00:00
_audit_creation_method                  'WinGX routine CIF_UPDATE'
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 4-dimethylamino-2-benzylidene malonic acid dimethyl ester
;
_chemical_formula_sum                   'C14 H17 N O4'
_chemical_formula_weight                263.29
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
 
_cell_length_a                          13.179(3)
_cell_length_b                          7.2410(19)
_cell_length_c                          15.270(4)
_cell_angle_alpha                       90
_cell_angle_beta                        101.580(3)
_cell_angle_gamma                       90
_cell_volume                            1427.5(6)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_density_diffrn           1.225
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    560
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.09
_exptl_absorpt_correction_type          none
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             293(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_av_R_equivalents         0.056
_diffrn_reflns_av_unetI/netI            0.0351
_diffrn_reflns_number                   14246
_diffrn_reflns_limit_h_min              -16
_diffrn_reflns_limit_h_max              16
_diffrn_reflns_limit_k_min              -8
_diffrn_reflns_limit_k_max              8
_diffrn_reflns_limit_l_min              -18
_diffrn_reflns_limit_l_max              18
_diffrn_reflns_theta_min                2.72
_diffrn_reflns_theta_max                25.82
_diffrn_reflns_theta_full               25.82
_diffrn_measured_fraction_theta_full
                                        0.997
_diffrn_measured_fraction_theta_max
                                        0.997
_reflns_number_total                    2739
_reflns_number_gt                       2138
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
 
#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
 
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0999P)²+0.2595P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                2739
_refine_ls_number_parameters            176
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0678
_refine_ls_R_factor_gt                  0.0547
_refine_ls_wR_factor_ref                0.1743
_refine_ls_wR_factor_gt                 0.1572
_refine_ls_goodness_of_fit_ref          1.043
_refine_ls_restrained_S_all             1.043
_refine_ls_shift/su_max                 0.076
_refine_ls_shift/su_mean                0.002
_refine_diff_density_max                0.215
_refine_diff_density_min                -0.253
_refine_diff_density_rms                0.042
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
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_symmetry_multiplicity
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_assembly
    _atom_site_disorder_group
C1 C 0.95400(14) 0.3323(2) 0.58316(12) 0.0533(4) Uani 1 1 d . . .
C2 C 1.05878(15) 0.2821(2) 0.58624(12) 0.0548(5) Uani 1 1 d . . .
H2 H 1.0776 0.2353 0.5351 0.066 Uiso 1 1 calc R . .
C3 C 1.13269(15) 0.3008(2) 0.66244(12) 0.0557(5) Uani 1 1 d . . .
H3 H 1.2003 0.2655 0.6616 0.067 Uiso 1 1 calc R . .
C4 C 1.10996(14) 0.3716(2) 0.74234(12) 0.0550(5) Uani 1 1 d . . .
C5 C 1.00707(15) 0.4286(2) 0.73754(12) 0.0573(5) Uani 1 1 d . . .
H5 H 0.9895 0.4819 0.7879 0.069 Uiso 1 1 calc R . .
C6 C 0.93179(15) 0.4094(2) 0.66253(13) 0.0586(5) Uani 1 1 d . . .
H6 H 0.8646 0.4477 0.6635 0.07 Uiso 1 1 calc R . .
C7 C 1.18056(16) 0.3832(3) 0.82722(12) 0.0604(5) Uani 1 1 d . . .
H7 H 1.1552 0.4491 0.8705 0.072 Uiso 1 1 calc R . .
C8 C 1.27662(15) 0.3159(3) 0.85530(12) 0.0611(5) Uani 1 1 d . . .
C9 C 1.32768(17) 0.3343(3) 0.95013(13) 0.0696(6) Uani 1 1 d . . .
C10 C 1.33616(14) 0.2148(4) 0.79620(13) 0.0680(6) Uani 1 1 d . . .
C11 C 1.4774(2) 0.2511(5) 1.05783(17) 0.1106(10) Uani 1 1 d . . .
H11A H 1.4903 0.376 1.0781 0.166 Uiso 1 1 calc R . .
H11B H 1.5421 0.188 1.0612 0.166 Uiso 1 1 calc R . .
H11C H 1.4374 0.189 1.0949 0.166 Uiso 1 1 calc R . .
C12 C 1.3670(2) -0.0756(5) 0.73629(17) 0.1034(10) Uani 1 1 d . . .
H12A H 1.3432 -0.0404 0.675 0.155 Uiso 1 1 calc R . .
H12B H 1.3519 -0.2038 0.7435 0.155 Uiso 1 1 calc R . .
H12C H 1.4404 -0.0561 0.7529 0.155 Uiso 1 1 calc R . .
C13 C 0.77371(18) 0.3682(4) 0.50502(18) 0.0845(7) Uani 1 1 d . . .
H13A H 0.7465 0.3067 0.551 0.127 Uiso 1 1 calc R . .
H13B H 0.7322 0.3379 0.4477 0.127 Uiso 1 1 calc R . .
H13C H 0.7724 0.4993 0.5141 0.127 Uiso 1 1 calc R . .
C14 C 0.90226(18) 0.2273(3) 0.42777(14) 0.0711(6) Uani 1 1 d . . .
H14A H 0.9526 0.3017 0.4066 0.107 Uiso 1 1 calc R . .
H14B H 0.84 0.2216 0.3827 0.107 Uiso 1 1 calc R . .
H14C H 0.9292 0.105 0.4405 0.107 Uiso 1 1 calc R . .
N N 0.87951(13) 0.3086(2) 0.50845(11) 0.0669(5) Uani 1 1 d . . .
O1 O 1.31492(10) 0.0355(2) 0.79303(9) 0.0713(4) Uani 1 1 d . . .
O2 O 1.39415(14) 0.2874(3) 0.75581(13) 0.1102(7) Uani 1 1 d . . .
O3 O 1.42049(12) 0.2516(3) 0.96598(10) 0.0888(5) Uani 1 1 d . . .
O4 O 1.29099(15) 0.4077(3) 1.00772(11) 0.0944(6) Uani 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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
C1 N 1.358(2) . ?
C1 C6 1.417(3) . ?
C1 C2 1.420(3) . ?
C2 C3 1.366(3) . ?
C3 C4 1.410(2) . ?
C4 C5 1.405(3) . ?
C4 C7 1.438(3) . ?
C5 C6 1.364(3) . ?
C7 C8 1.344(3) . ?
C8 C9 1.475(3) . ?
C8 C10 1.500(3) . ?
C9 O4 1.208(3) . ?
C9 O3 1.340(3) . ?
C10 O2 1.196(3) . ?
C10 O1 1.327(3) . ?
C11 O3 1.451(3) . ?
C12 O1 1.452(3) . ?
C13 N 1.450(3) . ?
C14 N 1.450(3) . ?
 
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
N C1 C6 121.98(17) . . ?
N C1 C2 121.98(16) . . ?
C6 C1 C2 116.04(17) . . ?
C3 C2 C1 121.71(16) . . ?
C2 C3 C4 122.27(17) . . ?
C5 C4 C3 115.61(17) . . ?
C5 C4 C7 118.22(16) . . ?
C3 C4 C7 126.12(17) . . ?
C6 C5 C4 123.07(16) . . ?
C5 C6 C1 121.20(17) . . ?
C8 C7 C4 131.62(18) . . ?
C7 C8 C9 119.69(18) . . ?
C7 C8 C10 123.91(18) . . ?
C9 C8 C10 116.37(18) . . ?
O4 C9 O3 123.3(2) . . ?
O4 C9 C8 125.7(2) . . ?
O3 C9 C8 110.91(18) . . ?
O2 C10 O1 124.3(2) . . ?
O2 C10 C8 124.1(2) . . ?
O1 C10 C8 111.56(16) . . ?
C1 N C14 121.82(17) . . ?
C1 N C13 121.34(17) . . ?
C14 N C13 116.82(18) . . ?
C10 O1 C12 116.2(2) . . ?
C9 O3 C11 116.83(19) . . ?








 
data_ele107
 
_audit_creation_date                    2011-06-23T10:59:57-00:00
_audit_creation_method                  'WinGX routine CIF_UPDATE'
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_sum                   'C16 H21 N O4'
_chemical_formula_weight                291.34
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
 
_cell_length_a                          14.7372(12)
_cell_length_b                          7.5331(6)
_cell_length_c                          15.9358(13)
_cell_angle_alpha                       90
_cell_angle_beta                        115.2660(10)
_cell_angle_gamma                       90
_cell_volume                            1599.9(2)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_density_diffrn           1.21
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    624
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.087
_exptl_absorpt_correction_type          none
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             293(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_av_R_equivalents         0.0221
_diffrn_reflns_av_unetI/netI            0.0173
_diffrn_reflns_number                   24862
_diffrn_reflns_limit_h_min              -21
_diffrn_reflns_limit_h_max              21
_diffrn_reflns_limit_k_min              -10
_diffrn_reflns_limit_k_max              10
_diffrn_reflns_limit_l_min              -22
_diffrn_reflns_limit_l_max              23
_diffrn_reflns_theta_min                1.53
_diffrn_reflns_theta_max                31.23
_diffrn_reflns_theta_full               31.23
_diffrn_measured_fraction_theta_full
                                        0.987
_diffrn_measured_fraction_theta_max
                                        0.987
_reflns_number_total                    5125
_reflns_number_gt                       3232
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
 
#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
 
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.1241P)²+0.2582P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                5125
_refine_ls_number_parameters            214
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0959
_refine_ls_R_factor_gt                  0.0632
_refine_ls_wR_factor_ref                0.2359
_refine_ls_wR_factor_gt                 0.1997
_refine_ls_goodness_of_fit_ref          1.035
_refine_ls_restrained_S_all             1.035
_refine_ls_shift/su_max                 0.114
_refine_ls_shift/su_mean                0.008
_refine_diff_density_max                0.503
_refine_diff_density_min                -0.271
_refine_diff_density_rms                0.077
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
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_symmetry_multiplicity
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_assembly
    _atom_site_disorder_group
C1 C 0.47940(12) 0.6777(2) 0.89253(11) 0.0540(4) Uani 1 1 d . . .
C2 C 0.44948(12) 0.6024(2) 0.80353(11) 0.0578(4) Uani 1 1 d . . .
H2 H 0.3838 0.5633 0.7709 0.069 Uiso 1 1 calc R . .
C3 C 0.51604(13) 0.5862(2) 0.76460(11) 0.0560(4) Uani 1 1 d . . .
H3 H 0.4943 0.5335 0.7065 0.067 Uiso 1 1 calc R . .
C4 C 0.61515(12) 0.6457(2) 0.80869(10) 0.0525(4) Uani 1 1 d . . .
C5 C 0.64539(12) 0.7161(2) 0.89820(11) 0.0548(4) Uani 1 1 d . . .
H5 H 0.7114 0.7537 0.9307 0.066 Uiso 1 1 calc R . .
C6 C 0.58073(12) 0.7312(2) 0.93917(11) 0.0548(4) Uani 1 1 d . . .
H6 H 0.604 0.7775 0.9988 0.066 Uiso 1 1 calc R . .
C7 C 0.67615(13) 0.6356(2) 0.75766(11) 0.0568(4) Uani 1 1 d . . .
H7 H 0.6483 0.5678 0.7038 0.068 Uiso 1 1 calc R . .
C8 C 0.76577(13) 0.7068(2) 0.77428(11) 0.0572(4) Uani 1 1 d . . .
C9 C 0.80382(15) 0.6838(3) 0.70230(14) 0.0670(5) Uani 1 1 d . . .
C10 C 0.82912(12) 0.8124(2) 0.85886(12) 0.0567(4) Uani 1 1 d . . .
C11' C 0.9638(11) 0.7809(18) 0.6850(11) 0.092(4) Uani 0.302(15) 1 d P . .
H11A H 1.0306 0.7964 0.7345 0.111 Uiso 0.302(15) 1 calc PR . .
H11B H 0.9615 0.6714 0.6521 0.111 Uiso 0.302(15) 1 calc PR . .
C11 C 0.9138(6) 0.7858(7) 0.6439(5) 0.0880(18) Uani 0.698(15) 1 d P . .
H11C H 0.9376 0.6696 0.6362 0.106 Uiso 0.698(15) 1 calc PR . .
H11D H 0.8577 0.8192 0.5863 0.106 Uiso 0.698(15) 1 calc PR . .
C12 C 0.85129(18) 1.0913(3) 0.93416(17) 0.0895(7) Uani 1 1 d . . .
H12A H 0.9216 1.0991 0.9465 0.107 Uiso 1 1 calc R . .
H12B H 0.8468 1.041 0.9883 0.107 Uiso 1 1 calc R . .
C13 C 0.30901(16) 0.6450(4) 0.88294(17) 0.0867(7) Uani 1 1 d . . .
H13A H 0.277 0.7165 0.8282 0.13 Uiso 1 1 calc R . .
H13B H 0.2761 0.6625 0.9229 0.13 Uiso 1 1 calc R . .
H13C H 0.3047 0.5222 0.8656 0.13 Uiso 1 1 calc R . .
C14 C 0.44364(18) 0.7671(3) 1.02391(15) 0.0790(6) Uani 1 1 d . . .
H14A H 0.5095 0.7246 1.0638 0.119 Uiso 1 1 calc R . .
H14B H 0.3968 0.7295 1.0476 0.119 Uiso 1 1 calc R . .
H14C H 0.4445 0.8944 1.0216 0.119 Uiso 1 1 calc R . .
C15' C 0.9342(14) 0.9291(16) 0.6242(11) 0.100(4) Uani 0.302(15) 1 d P . .
H15A H 0.8691 0.9073 0.5749 0.15 Uiso 0.302(15) 1 calc PR . .
H15B H 0.9819 0.9471 0.5987 0.15 Uiso 0.302(15) 1 calc PR . .
H15C H 0.9317 1.033 0.658 0.15 Uiso 0.302(15) 1 calc PR . .
C15 C 0.9953(8) 0.9188(12) 0.6701(7) 0.152(4) Uani 0.698(15) 1 d P . .
H15D H 0.9674 1.0359 0.6631 0.229 Uiso 0.698(15) 1 calc PR . .
H15E H 1.0293 0.9059 0.6307 0.229 Uiso 0.698(15) 1 calc PR . .
H15F H 1.0422 0.9006 0.7336 0.229 Uiso 0.698(15) 1 calc PR . .
C16 C 0.8054(2) 1.2690(4) 0.9147(2) 0.1122(10) Uani 1 1 d . . .
H16A H 0.8084 1.3162 0.86 0.168 Uiso 1 1 calc R . .
H16B H 0.8412 1.346 0.9663 0.168 Uiso 1 1 calc R . .
H16C H 0.7366 1.2607 0.905 0.168 Uiso 1 1 calc R . .
N N 0.41371(13) 0.6961(3) 0.93150(12) 0.0753(5) Uani 1 1 d . . .
O1 O 0.79763(9) 0.97892(17) 0.85313(9) 0.0669(4) Uani 1 1 d . . .
O2 O 0.89905(10) 0.7534(2) 0.92473(10) 0.0804(4) Uani 1 1 d . . .
O3 O 0.88369(13) 0.7848(2) 0.72162(12) 0.0900(5) Uani 1 1 d . . .
O4 O 0.76670(13) 0.5918(2) 0.63411(11) 0.0897(5) Uani 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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
C1 N 1.362(2) . ?
C1 C2 1.412(2) . ?
C1 C6 1.413(2) . ?
C2 C3 1.372(2) . ?
C3 C4 1.397(2) . ?
C4 C5 1.404(2) . ?
C4 C7 1.449(2) . ?
C5 C6 1.370(2) . ?
C7 C8 1.343(2) . ?
C8 C9 1.486(3) . ?
C8 C10 1.499(2) . ?
C9 O4 1.206(3) . ?
C9 O3 1.323(3) . ?
C10 O2 1.199(2) . ?
C10 O1 1.327(2) . ?
C11' C15' 1.419(19) . ?
C11' O3 1.524(10) . ?
C11 C15 1.481(9) . ?
C11 O3 1.484(4) . ?
C12 O1 1.462(3) . ?
C12 C16 1.472(4) . ?
C13 N 1.452(3) . ?
C14 N 1.447(3) . ?
 
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
N C1 C2 121.39(15) . . ?
N C1 C6 121.88(15) . . ?
C2 C1 C6 116.72(15) . . ?
C3 C2 C1 120.87(15) . . ?
C2 C3 C4 122.68(14) . . ?
C3 C4 C5 116.25(15) . . ?
C3 C4 C7 117.83(14) . . ?
C5 C4 C7 125.88(15) . . ?
C6 C5 C4 122.11(15) . . ?
C5 C6 C1 121.28(14) . . ?
C8 C7 C4 131.45(16) . . ?
C7 C8 C9 117.68(17) . . ?
C7 C8 C10 124.88(16) . . ?
C9 C8 C10 117.41(16) . . ?
O4 C9 O3 123.84(19) . . ?
O4 C9 C8 125.96(19) . . ?
O3 C9 C8 110.17(17) . . ?
O2 C10 O1 123.73(17) . . ?
O2 C10 C8 124.27(17) . . ?
O1 C10 C8 111.99(14) . . ?
C15' C11' O3 100.6(10) . . ?
C15 C11 O3 105.3(5) . . ?
O1 C12 C16 108.27(19) . . ?
C1 N C14 122.29(16) . . ?
C1 N C13 122.02(16) . . ?
C14 N C13 115.68(17) . . ?
C10 O1 C12 116.43(15) . . ?
C9 O3 C11 111.2(3) . . ?
C9 O3 C11' 131.1(6) . . ?
C11 O3 C11' 28.8(4) . . ?





data_ele108
 
_audit_creation_date                    2011-06-23T10:58:55-00:00
_audit_creation_method                  'WinGX routine CIF_UPDATE'
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_sum                   'C16 H21 N O4'
_chemical_formula_weight                291.34
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
 
_cell_length_a                          23.263(3)
_cell_length_b                          7.8210(10)
_cell_length_c                          19.649(2)
_cell_angle_alpha                       90
_cell_angle_beta                        116.6140(17)
_cell_angle_gamma                       90
_cell_volume                            3196.2(7)
_cell_formula_units_Z                   8
_cell_measurement_temperature           293(2)
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_density_diffrn           1.211
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1248
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.087
_exptl_absorpt_correction_type          none
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             293(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_av_R_equivalents         0.0371
_diffrn_reflns_av_unetI/netI            0.028
_diffrn_reflns_number                   21837
_diffrn_reflns_limit_h_min              -31
_diffrn_reflns_limit_h_max              31
_diffrn_reflns_limit_k_min              -10
_diffrn_reflns_limit_k_max              10
_diffrn_reflns_limit_l_min              -26
_diffrn_reflns_limit_l_max              26
_diffrn_reflns_theta_min                1.96
_diffrn_reflns_theta_max                28.63
_diffrn_reflns_theta_full               28.63
_diffrn_measured_fraction_theta_full
                                        0.999
_diffrn_measured_fraction_theta_max
                                        0.999
_reflns_number_total                    4111
_reflns_number_gt                       2449
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
 
#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
 
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          geom
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0622P)²+0.7405P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                4111
_refine_ls_number_parameters            194
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0888
_refine_ls_R_factor_gt                  0.0464
_refine_ls_wR_factor_ref                0.1378
_refine_ls_wR_factor_gt                 0.1164
_refine_ls_goodness_of_fit_ref          1.016
_refine_ls_restrained_S_all             1.016
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.147
_refine_diff_density_min                -0.148
_refine_diff_density_rms                0.031
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
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_symmetry_multiplicity
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_disorder_assembly
    _atom_site_disorder_group
C1 C 0.16963(8) 0.2991(2) 0.75521(9) 0.0525(4) Uani 1 1 d . . .
C2 C 0.11689(8) 0.2178(2) 0.69569(9) 0.0590(4) Uani 1 1 d . . .
H2 H 0.0846 0.1714 0.7056 0.071 Uiso 1 1 calc R . .
C3 C 0.11194(8) 0.2054(2) 0.62353(9) 0.0534(4) Uani 1 1 d . . .
H3 H 0.0763 0.1511 0.5859 0.064 Uiso 1 1 calc R . .
C4 C 0.15897(7) 0.27203(19) 0.60524(8) 0.0466(3) Uani 1 1 d . . .
C5 C 0.21097(7) 0.3526(2) 0.66439(8) 0.0531(4) Uani 1 1 d . . .
H5 H 0.2435 0.3973 0.6544 0.064 Uiso 1 1 calc R . .
C6 C 0.21624(7) 0.3685(2) 0.73634(9) 0.0563(4) Uani 1 1 d . . .
H6 H 0.2513 0.4263 0.7733 0.068 Uiso 1 1 calc R . .
C7 C 0.15875(7) 0.26122(19) 0.53149(8) 0.0474(4) Uani 1 1 d . . .
H7 H 0.1984 0.2828 0.5325 0.057 Uiso 1 1 calc R . .
C8 C 0.11157(7) 0.22568(19) 0.46194(8) 0.0463(3) Uani 1 1 d . . .
C9 C 0.12803(7) 0.2245(2) 0.39776(8) 0.0517(4) Uani 1 1 d . . .
C10 C 0.04313(7) 0.1897(2) 0.44378(8) 0.0480(4) Uani 1 1 d . . .
C11 C 0.08701(10) 0.2507(3) 0.26406(10) 0.0811(6) Uani 1 1 d . . .
H11A H 0.0469 0.243 0.2189 0.122 Uiso 0.67(2) 1 calc PR . .
H11B H 0.1152 0.1612 0.2639 0.122 Uiso 0.67(2) 1 calc PR . .
H11C H 0.1065 0.3597 0.2654 0.122 Uiso 0.67(2) 1 calc PR . .
H11D H 0.1322 0.2663 0.2799 0.122 Uiso 0.33(2) 1 calc PR . .
H11E H 0.0638 0.3481 0.2349 0.122 Uiso 0.33(2) 1 calc PR . .
H11F H 0.0725 0.1496 0.2334 0.122 Uiso 0.33(2) 1 calc PR . .
C12 C -0.05188(8) 0.3051(3) 0.44003(13) 0.0817(6) Uani 1 1 d . . .
H12A H -0.0551 0.3387 0.4852 0.123 Uiso 0.29(3) 1 calc PR . .
H12B H -0.0639 0.1872 0.4291 0.123 Uiso 0.29(3) 1 calc PR . .
H12C H -0.0801 0.3746 0.398 0.123 Uiso 0.29(3) 1 calc PR . .
H12D H -0.0776 0.2616 0.3897 0.123 Uiso 0.71(3) 1 calc PR . .
H12E H -0.0688 0.4131 0.4457 0.123 Uiso 0.71(3) 1 calc PR . .
H12F H -0.0527 0.2257 0.4769 0.123 Uiso 0.71(3) 1 calc PR . .
C13 C 0.23062(9) 0.3926(2) 0.88828(9) 0.0686(5) Uani 1 1 d . . .
H13A H 0.2191 0.4271 0.928 0.082 Uiso 1 1 calc R . .
H13B H 0.2406 0.4954 0.868 0.082 Uiso 1 1 calc R . .
C14 C 0.13455(12) 0.2106(3) 0.85175(11) 0.0839(7) Uani 1 1 d . . .
H14A H 0.161 0.1632 0.9018 0.101 Uiso 1 1 calc R . .
H14B H 0.1162 0.1157 0.8169 0.101 Uiso 1 1 calc R . .
C15 C 0.29013(11) 0.2820(3) 0.92311(12) 0.0917(7) Uani 1 1 d . . .
H15A H 0.3245 0.3453 0.962 0.138 Uiso 1 1 calc R . .
H15B H 0.3024 0.2488 0.8844 0.138 Uiso 1 1 calc R . .
H15C H 0.2813 0.1818 0.945 0.138 Uiso 1 1 calc R . .
C16 C 0.08119(14) 0.3109(4) 0.85494(18) 0.1218(10) Uani 1 1 d . . .
H16A H 0.0567 0.238 0.8714 0.183 Uiso 1 1 calc R . .
H16B H 0.0538 0.3553 0.8053 0.183 Uiso 1 1 calc R . .
H16C H 0.0988 0.4039 0.8902 0.183 Uiso 1 1 calc R . .
N N 0.17536(7) 0.30929(19) 0.82772(8) 0.0669(4) Uani 1 1 d . . .
O1 O 0.01369(5) 0.32769(15) 0.45176(7) 0.0635(3) Uani 1 1 d . . .
O2 O 0.01791(5) 0.05360(16) 0.42389(7) 0.0716(4) Uani 1 1 d . . .
O3 O 0.07572(5) 0.23317(16) 0.33043(6) 0.0655(3) Uani 1 1 d . . .
O4 O 0.18155(5) 0.2212(2) 0.40337(7) 0.0757(4) Uani 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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
C1 N 1.373(2) . ?
C1 C6 1.403(2) . ?
C1 C2 1.411(2) . ?
C2 C3 1.374(2) . ?
C3 C4 1.396(2) . ?
C4 C5 1.397(2) . ?
C4 C7 1.449(2) . ?
C5 C6 1.369(2) . ?
C7 C8 1.344(2) . ?
C8 C9 1.473(2) . ?
C8 C10 1.494(2) . ?
C9 O4 1.1999(18) . ?
C9 O3 1.3392(18) . ?
C10 O2 1.1931(18) . ?
C10 O1 1.3248(19) . ?
C11 O3 1.448(2) . ?
C12 O1 1.4478(19) . ?
C13 N 1.457(2) . ?
C13 C15 1.511(3) . ?
C14 N 1.457(2) . ?
C14 C16 1.494(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
N C1 C6 121.66(14) . . ?
N C1 C2 122.04(15) . . ?
C6 C1 C2 116.30(14) . . ?
C3 C2 C1 121.81(15) . . ?
C2 C3 C4 121.74(14) . . ?
C3 C4 C5 116.14(13) . . ?
C3 C4 C7 125.68(13) . . ?
C5 C4 C7 118.16(13) . . ?
C6 C5 C4 122.95(14) . . ?
C5 C6 C1 121.03(14) . . ?
C8 C7 C4 131.63(14) . . ?
C7 C8 C9 117.70(13) . . ?
C7 C8 C10 125.40(13) . . ?
C9 C8 C10 116.89(12) . . ?
O4 C9 O3 122.56(15) . . ?
O4 C9 C8 125.34(14) . . ?
O3 C9 C8 112.07(13) . . ?
O2 C10 O1 124.14(14) . . ?
O2 C10 C8 124.14(15) . . ?
O1 C10 C8 111.72(13) . . ?
N C13 C15 114.06(16) . . ?
N C14 C16 114.19(19) . . ?
C1 N C14 122.10(14) . . ?
C1 N C13 120.91(14) . . ?
C14 N C13 115.92(14) . . ?
C10 O1 C12 116.45(14) . . ?
C9 O3 C11 116.33(13) . . ?
 
# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./
 
# END of CIF
