 
data_test1
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C24 H26 N2 O7' 
_chemical_formula_weight          454.47 
 
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'   0.0000   0.0000 
 '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   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'Triclinic' 
_symmetry_space_group_name_H-M    'P-1   ' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    8.25(2) 
_cell_length_b                    10.46(2) 
_cell_length_c                    13.93(3) 
_cell_angle_alpha                 77.91(4) 
_cell_angle_beta                  76.47(4) 
_cell_angle_gamma                 85.92(4) 
_cell_volume                      1142(5) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     1079 
_cell_measurement_theta_min       2.54 
_cell_measurement_theta_max       20.75 
 
_exptl_crystal_description        'Needle' 
_exptl_crystal_colour             'Color less' 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.321 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              480 
_exptl_absorpt_coefficient_mu     0.098 
_exptl_absorpt_correction_type    'Multi-Scan' 
_exptl_absorpt_correction_T_min   0.9712 
_exptl_absorpt_correction_T_max   0.9903 
_exptl_absorpt_process_details    'Sadabs' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             3415 
_diffrn_reflns_av_R_equivalents   0.0399 
_diffrn_reflns_av_sigmaI/netI     0.0797 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          1.53 
_diffrn_reflns_theta_max          21.56 
_reflns_number_total              2381 
_reflns_number_gt                 1623 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker APEX2' 
_computing_cell_refinement        'Bruker SAINT' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'Mercury 3.8' 
_computing_publication_material   'Ortep 3v.2' 
 
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.09(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2381 
_refine_ls_number_parameters      300 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1863 
_refine_ls_R_factor_gt            0.1576 
_refine_ls_wR_factor_ref          0.4746 
_refine_ls_wR_factor_gt           0.4564 
_refine_ls_goodness_of_fit_ref    1.845 
_refine_ls_restrained_S_all       1.845 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 
C5 C 0.5127(14) 0.1599(12) 0.6930(9) 0.052(3) Uani 1 1 d . . . 
C3 C 0.7000(14) -0.0078(12) 0.6311(9) 0.049(3) Uani 1 1 d . . . 
C6 C 0.5468(15) 0.1158(12) 0.7883(9) 0.053(3) Uani 1 1 d . . . 
H6 H 0.4949 0.1550 0.8420 0.063 Uiso 1 1 calc R . . 
C1 C 0.6574(14) 0.0142(12) 0.8008(9) 0.050(3) Uani 1 1 d . . . 
C2 C 0.7364(15) -0.0499(12) 0.7249(9) 0.057(4) Uani 1 1 d . . . 
H2 H 0.8114 -0.1190 0.7365 0.068 Uiso 1 1 calc R . . 
C4 C 0.5909(14) 0.0984(12) 0.6124(9) 0.050(3) Uani 1 1 d . . . 
H4 H 0.5703 0.1278 0.5485 0.060 Uiso 1 1 calc R . . 
N2 N 0.7890(14) -0.0627(10) 0.5452(9) 0.060(3) Uani 1 1 d . . . 
N1 N 0.6983(14) -0.0310(14) 0.9030(9) 0.072(4) Uani 1 1 d . . . 
O4 O 0.7418(11) -0.0374(8) 0.4665(7) 0.066(3) Uani 1 1 d . . . 
O3 O 0.9094(12) -0.1359(9) 0.5565(7) 0.071(3) Uani 1 1 d . . . 
O1 O 0.7623(15) -0.1390(12) 0.9195(8) 0.103(4) Uani 1 1 d . . . 
O2 O 0.6689(14) 0.0467(13) 0.9615(8) 0.096(4) Uani 1 1 d . . . 
C7 C 0.3981(14) 0.2744(11) 0.6757(9) 0.044(3) Uani 1 1 d . . . 
O5 O 0.3618(11) 0.3182(9) 0.5943(6) 0.063(3) Uani 1 1 d . . . 
O6 O 0.3407(9) 0.3209(7) 0.7601(5) 0.048(2) Uani 1 1 d . . . 
C8 C 0.2043(13) 0.4200(11) 0.7664(8) 0.041(3) Uani 1 1 d . . . 
H8 H 0.1981 0.4658 0.6984 0.049 Uiso 1 1 calc R . . 
C9 C 0.2487(14) 0.5173(12) 0.8246(8) 0.046(3) Uani 1 1 d . . . 
C13 C 0.3916(15) 0.6180(12) 0.7636(8) 0.047(3) Uani 1 1 d . . . 
C14 C 0.2951(17) 0.7517(12) 0.7706(9) 0.057(4) Uani 1 1 d . . . 
H14 H 0.3664 0.8274 0.7571 0.068 Uiso 1 1 calc R . . 
C11 C 0.5087(15) 0.4543(12) 0.8821(9) 0.055(4) Uani 1 1 d . . . 
H11A H 0.5596 0.4399 0.9397 0.065 Uiso 1 1 calc R . . 
H11B H 0.5571 0.3924 0.8396 0.065 Uiso 1 1 calc R . . 
C16 C 0.1003(16) 0.6119(12) 0.8558(8) 0.053(4) Uani 1 1 d . . . 
H16 H 0.0086 0.5725 0.9102 0.063 Uiso 1 1 calc R . . 
C12 C 0.5311(15) 0.5944(12) 0.8234(9) 0.053(4) Uani 1 1 d . . . 
H12A H 0.6403 0.6047 0.7781 0.064 Uiso 1 1 calc R . . 
H12B H 0.5187 0.6550 0.8688 0.064 Uiso 1 1 calc R . . 
C10 C 0.3194(14) 0.4417(11) 0.9155(7) 0.045(3) Uani 1 1 d . . . 
H10A H 0.2764 0.4798 0.9745 0.054 Uiso 1 1 calc R . . 
H10B H 0.2890 0.3506 0.9316 0.054 Uiso 1 1 calc R . . 
C15 C 0.1824(17) 0.7227(13) 0.8762(10) 0.066(4) Uani 1 1 d . . . 
H15A H 0.2442 0.6957 0.9287 0.080 Uiso 1 1 calc R . . 
H15B H 0.1056 0.7943 0.8907 0.080 Uiso 1 1 calc R . . 
C17 C 0.4684(15) 0.6080(12) 0.6541(8) 0.048(3) Uani 1 1 d . . . 
H17A H 0.5310 0.5262 0.6519 0.058 Uiso 1 1 calc R . . 
H17B H 0.3811 0.6102 0.6177 0.058 Uiso 1 1 calc R . . 
O7 O 0.5769(14) 0.7159(10) 0.6085(6) 0.083(3) Uani 1 1 d . . . 
H7 H 0.6125 0.7151 0.5485 0.124 Uiso 1 1 calc R . . 
C18 C 0.1700(18) 0.7650(12) 0.7076(10) 0.058(4) Uani 1 1 d . . . 
H18 H 0.1740 0.8202 0.6455 0.069 Uiso 1 1 calc R . . 
C20 C 0.0177(17) 0.2374(14) 0.7641(12) 0.065(4) Uani 1 1 d . . . 
C19 C 0.0424(15) 0.3473(13) 0.8170(9) 0.061(4) Uani 1 1 d . . . 
H19A H -0.0512 0.4089 0.8164 0.073 Uiso 1 1 calc R . . 
H19B H 0.0438 0.3102 0.8867 0.073 Uiso 1 1 calc R . . 
C21 C -0.045(2) 0.2717(19) 0.6738(14) 0.089(5) Uani 1 1 d . . . 
H21 H -0.0411 0.2042 0.6392 0.107 Uiso 1 1 calc R . . 
C23 C 0.062(2) 0.1159(16) 0.7957(16) 0.105(6) Uani 1 1 d . . . 
H23A H 0.0524 0.0523 0.7597 0.126 Uiso 1 1 calc R . . 
H23B H 0.1022 0.0932 0.8541 0.126 Uiso 1 1 calc R . . 
C22 C -0.106(2) 0.384(2) 0.6324(15) 0.110(6) Uani 1 1 d . . . 
H22A H -0.1138 0.4560 0.6626 0.132 Uiso 1 1 calc R . . 
H22B H -0.1419 0.3908 0.5729 0.132 Uiso 1 1 calc R . . 
C24 C 0.0509(17) 0.6814(15) 0.7587(10) 0.065(4) Uani 1 1 d . . . 
H24 H -0.0454 0.6677 0.7387 0.078 Uiso 1 1 calc R . . 
 
 
_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 
C5 C6 1.397(17) . ? 
C5 C4 1.413(17) . ? 
C5 C7 1.487(16) . ? 
C3 C2 1.384(17) . ? 
C3 C4 1.400(16) . ? 
C3 N2 1.456(15) . ? 
C6 C1 1.361(16) . ? 
C1 C2 1.380(17) . ? 
C1 N1 1.511(16) . ? 
N2 O4 1.219(13) . ? 
N2 O3 1.230(13) . ? 
N1 O1 1.213(14) . ? 
N1 O2 1.241(15) . ? 
C7 O5 1.227(13) . ? 
C7 O6 1.337(13) . ? 
O6 C8 1.475(12) . ? 
C8 C19 1.529(16) . ? 
C8 C9 1.538(16) . ? 
C9 C16 1.557(16) . ? 
C9 C10 1.559(15) . ? 
C9 C13 1.599(17) . ? 
C13 C17 1.530(15) . ? 
C13 C12 1.549(17) . ? 
C13 C14 1.569(17) . ? 
C14 C18 1.485(18) . ? 
C14 C15 1.528(17) . ? 
C11 C12 1.522(17) . ? 
C11 C10 1.528(16) . ? 
C16 C15 1.491(19) . ? 
C16 C24 1.527(17) . ? 
C17 O7 1.434(14) . ? 
C18 C24 1.331(18) . ? 
C20 C23 1.31(2) . ? 
C20 C21 1.44(2) . ? 
C20 C19 1.538(19) . ? 
C21 C22 1.32(2) . ? 
 
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 
C6 C5 C4 120.1(11) . . ? 
C6 C5 C7 119.9(11) . . ? 
C4 C5 C7 119.9(11) . . ? 
C2 C3 C4 121.6(10) . . ? 
C2 C3 N2 120.8(11) . . ? 
C4 C3 N2 117.2(11) . . ? 
C1 C6 C5 118.6(12) . . ? 
C6 C1 C2 123.8(11) . . ? 
C6 C1 N1 118.6(12) . . ? 
C2 C1 N1 117.6(11) . . ? 
C1 C2 C3 117.6(11) . . ? 
C3 C4 C5 118.4(11) . . ? 
O4 N2 O3 122.6(10) . . ? 
O4 N2 C3 120.1(11) . . ? 
O3 N2 C3 117.3(11) . . ? 
O1 N1 O2 125.5(12) . . ? 
O1 N1 C1 116.9(13) . . ? 
O2 N1 C1 117.5(12) . . ? 
O5 C7 O6 125.5(10) . . ? 
O5 C7 C5 123.6(10) . . ? 
O6 C7 C5 110.9(10) . . ? 
C7 O6 C8 120.9(8) . . ? 
O6 C8 C19 107.1(9) . . ? 
O6 C8 C9 106.7(9) . . ? 
C19 C8 C9 114.7(9) . . ? 
C8 C9 C16 112.5(10) . . ? 
C8 C9 C10 109.8(10) . . ? 
C16 C9 C10 113.0(9) . . ? 
C8 C9 C13 116.0(8) . . ? 
C16 C9 C13 101.5(9) . . ? 
C10 C9 C13 103.7(9) . . ? 
C17 C13 C12 108.7(10) . . ? 
C17 C13 C14 111.5(9) . . ? 
C12 C13 C14 112.8(10) . . ? 
C17 C13 C9 116.9(10) . . ? 
C12 C13 C9 106.0(9) . . ? 
C14 C13 C9 100.7(9) . . ? 
C18 C14 C15 100.8(11) . . ? 
C18 C14 C13 107.6(10) . . ? 
C15 C14 C13 102.3(9) . . ? 
C12 C11 C10 103.5(10) . . ? 
C15 C16 C24 98.7(11) . . ? 
C15 C16 C9 103.5(11) . . ? 
C24 C16 C9 106.4(9) . . ? 
C11 C12 C13 104.7(9) . . ? 
C11 C10 C9 105.8(8) . . ? 
C16 C15 C14 93.6(11) . . ? 
O7 C17 C13 108.7(9) . . ? 
C24 C18 C14 105.7(11) . . ? 
C23 C20 C21 119.7(16) . . ? 
C23 C20 C19 121.7(16) . . ? 
C21 C20 C19 118.4(13) . . ? 
C8 C19 C20 112.3(10) . . ? 
C22 C21 C20 130.1(18) . . ? 
C18 C24 C16 107.9(12) . . ? 
 
_diffrn_measured_fraction_theta_max    0.899 
_diffrn_reflns_theta_full              21.56 
_diffrn_measured_fraction_theta_full   0.899 
_refine_diff_density_max    0.584 
_refine_diff_density_min   -0.638 
_refine_diff_density_rms    0.154
# start Validation Reply Form
_vrf_THETM01_test1           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength =    0.5170
RESPONSE:The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
_vrf_PLAT029_test1
;
PROBLEM:diffrn_measured_fraction_theta_full value Low .      0.899 Why? 
RESPONSE:The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
_vrf_PLAT084_test1
;
PROBLEM:High wR2 Value (i.e. > 0.25) ...................0.47 Report
RESPONSE:The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
_vrf_REFNR01_test1
;
PROBLEM:Ratio of reflections to parameters is < 8 for a centrosymmetric structure  sine(theta)/lambda 0.5170
            Proportion of unique data used    1.0000
            Ratio reflections to parameters   7.9367
RESPONSE:The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
_vrf_PLAT082_test1
;
PROBLEM:High R1 Value ..................................       0.16 Report
RESPONSE:The crystal was poorly diffracting at higher Bragg angles.
The situation did not improve even after recrystallisation and fresh
data collection.
;
# end Validation Reply Form
 
