 
data_cdwtd30_0m_a
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C18 H17 N' 
_chemical_formula_weight          247.32

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'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            148
_space_group_name_H-M_alt         'R -3 :H'
_space_group_name_Hall            '-R 3'
 
_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'
 '-y, x-y, z'
 '-x+y, -x, z'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 
_cell_length_a                    31.023(7)
_cell_length_b                    31.023(7)
_cell_length_c                    7.2503(14)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      6043(3)
_cell_formula_units_Z             18
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.223          
_exptl_crystal_F_000              2376
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.547
_exptl_crystal_size_mid           0.152
_exptl_crystal_size_min           0.145
_exptl_absorpt_coefficient_mu     0.071
_shelx_estimated_absorpt_T_min    0.962
_shelx_estimated_absorpt_T_max    0.990
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             12700
_diffrn_reflns_av_unetI/netI      0.0488
_diffrn_reflns_av_R_equivalents   0.0607
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        34
_diffrn_reflns_limit_k_min        -34
_diffrn_reflns_limit_k_max        32
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          2.274
_diffrn_reflns_theta_max          23.279
_diffrn_reflns_theta_full         23.279
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              1923
_reflns_number_gt                 1351
_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     ?
_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)+(0.1000P)²+0.0307P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_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        0.0034(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1923
_refine_ls_number_parameters      173
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0864
_refine_ls_R_factor_gt            0.0524
_refine_ls_wR_factor_ref          0.1443
_refine_ls_wR_factor_gt           0.1272
_refine_ls_goodness_of_fit_ref    0.952
_refine_ls_restrained_S_all       0.952
_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_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
N001 N 0.03077(7) 0.45224(8) 0.4578(3) 0.0440(6) Uani 1 1 d . . . . .
C002 C 0.10277(9) 0.44744(8) 0.4099(3) 0.0342(6) Uani 1 1 d . . . . .
C003 C 0.15784(9) 0.53666(8) 0.4936(3) 0.0359(6) Uani 1 1 d . . . . .
C004 C 0.11468(9) 0.48623(8) 0.5569(3) 0.0338(6) Uani 1 1 d . . . . .
C005 C 0.05362(9) 0.42936(8) 0.3565(3) 0.0368(6) Uani 1 1 d . . . . .
C006 C 0.06484(9) 0.48457(9) 0.5650(3) 0.0384(6) Uani 1 1 d . . . . .
C007 C 0.13120(9) 0.43047(9) 0.3239(3) 0.0414(7) Uani 1 1 d . . . . .
H007 H 0.1641 0.4424 0.3583 0.050 Uiso 1 1 calc R U . . .
C008 C 0.12191(9) 0.47010(9) 0.7513(3) 0.0417(7) Uani 1 1 d . . . . .
H00A H 0.0969 0.4356 0.7719 0.050 Uiso 1 1 calc R U . . .
H00B H 0.1544 0.4727 0.7582 0.050 Uiso 1 1 calc R U . . .
C009 C 0.14926(10) 0.56563(9) 0.3692(3) 0.0460(7) Uani 1 1 d . . . . .
H009 H 0.1168 0.5554 0.3323 0.055 Uiso 1 1 calc R U . . .
C00A C 0.20651(9) 0.55313(10) 0.5442(3) 0.0459(7) Uani 1 1 d . . . . .
H00C H 0.2134 0.5344 0.6266 0.055 Uiso 1 1 calc R U . . .
C00B C 0.11785(10) 0.50226(9) 0.9006(3) 0.0469(7) Uani 1 1 d . . . . .
H00D H 0.1230 0.4915 1.0202 0.056 Uiso 1 1 calc R U . . .
H00E H 0.1438 0.5366 0.8827 0.056 Uiso 1 1 calc R U . . .
C00C C 0.05650(10) 0.51380(10) 0.7087(3) 0.0488(7) Uani 1 1 d . . . . .
H00F H 0.0223 0.5067 0.7041 0.059 Uiso 1 1 calc R U . . .
H00G H 0.0783 0.5491 0.6875 0.059 Uiso 1 1 calc R U . . .
C00D C 0.10958(11) 0.39529(9) 0.1852(3) 0.0488(7) Uani 1 1 d . . . . .
H00H H 0.1283 0.3836 0.1258 0.059 Uiso 1 1 calc R U . . .
C00E C 0.03196(10) 0.39395(9) 0.2193(3) 0.0460(7) Uani 1 1 d . . . . .
H00I H -0.0011 0.3816 0.1852 0.055 Uiso 1 1 calc R U . . .
C00F C 0.06090(11) 0.37741(9) 0.1342(3) 0.0502(8) Uani 1 1 d . . . . .
H00J H 0.0472 0.3538 0.0408 0.060 Uiso 1 1 calc R U . . .
C00G C 0.18778(12) 0.60916(10) 0.2997(3) 0.0541(8) Uani 1 1 d . . . . .
H00K H 0.1812 0.6279 0.2164 0.065 Uiso 1 1 calc R U . . .
C00H C 0.06749(10) 0.49923(10) 0.8983(3) 0.0496(7) Uani 1 1 d . . . . .
H00L H 0.0669 0.5213 0.9917 0.060 Uiso 1 1 calc R U . . .
H00M H 0.0418 0.4656 0.9281 0.060 Uiso 1 1 calc R U . . .
C00I C 0.23596(11) 0.62504(10) 0.3525(4) 0.0561(8) Uani 1 1 d . . . . .
H00N H 0.2621 0.6545 0.3059 0.067 Uiso 1 1 calc R U . . .
C00J C 0.24500(10) 0.59680(11) 0.4748(4) 0.0556(8) Uani 1 1 d . . . . .
H00O H 0.2775 0.6072 0.5113 0.067 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
N001 C006 1.291(3) . ?
N001 C005 1.432(3) . ?
C002 C007 1.381(3) . ?
C002 C005 1.391(3) . ?
C002 C004 1.509(3) . ?
C003 C00A 1.380(3) . ?
C003 C009 1.389(3) . ?
C003 C004 1.535(3) . ?
C004 C006 1.522(3) . ?
C004 C008 1.549(3) . ?
C005 C00E 1.382(3) . ?
C006 C00C 1.486(3) . ?
C007 C00D 1.386(3) . ?
C007 H007 0.9300 . ?
C008 C00B 1.520(3) . ?
C008 H00A 0.9700 . ?
C008 H00B 0.9700 . ?
C009 C00G 1.376(4) . ?
C009 H009 0.9300 . ?
C00A C00J 1.377(4) . ?
C00A H00C 0.9300 . ?
C00B C00H 1.518(3) . ?
C00B H00D 0.9700 . ?
C00B H00E 0.9700 . ?
C00C C00H 1.538(3) . ?
C00C H00F 0.9700 . ?
C00C H00G 0.9700 . ?
C00D C00F 1.374(4) . ?
C00D H00H 0.9300 . ?
C00E C00F 1.382(4) . ?
C00E H00I 0.9300 . ?
C00F H00J 0.9300 . ?
C00G C00I 1.374(4) . ?
C00G H00K 0.9300 . ?
C00H H00L 0.9700 . ?
C00H H00M 0.9700 . ?
C00I C00J 1.370(4) . ?
C00I H00N 0.9300 . ?
C00J H00O 0.9300 . ?
 
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
C006 N001 C005 106.13(19) . . ?
C007 C002 C005 120.1(2) . . ?
C007 C002 C004 132.4(2) . . ?
C005 C002 C004 107.5(2) . . ?
C00A C003 C009 117.5(2) . . ?
C00A C003 C004 122.2(2) . . ?
C009 C003 C004 120.1(2) . . ?
C002 C004 C006 99.25(18) . . ?
C002 C004 C003 110.01(17) . . ?
C006 C004 C003 113.54(18) . . ?
C002 C004 C008 113.74(18) . . ?
C006 C004 C008 105.23(18) . . ?
C003 C004 C008 114.10(18) . . ?
C00E C005 C002 121.3(2) . . ?
C00E C005 N001 126.8(2) . . ?
C002 C005 N001 111.9(2) . . ?
N001 C006 C00C 124.8(2) . . ?
N001 C006 C004 115.2(2) . . ?
C00C C006 C004 119.4(2) . . ?
C002 C007 C00D 118.6(2) . . ?
C002 C007 H007 120.7 . . ?
C00D C007 H007 120.7 . . ?
C00B C008 C004 111.29(19) . . ?
C00B C008 H00A 109.4 . . ?
C004 C008 H00A 109.4 . . ?
C00B C008 H00B 109.4 . . ?
C004 C008 H00B 109.4 . . ?
H00A C008 H00B 108.0 . . ?
C00G C009 C003 121.3(3) . . ?
C00G C009 H009 119.3 . . ?
C003 C009 H009 119.3 . . ?
C00J C00A C003 121.1(2) . . ?
C00J C00A H00C 119.4 . . ?
C003 C00A H00C 119.4 . . ?
C00H C00B C008 111.9(2) . . ?
C00H C00B H00D 109.2 . . ?
C008 C00B H00D 109.2 . . ?
C00H C00B H00E 109.2 . . ?
C008 C00B H00E 109.2 . . ?
H00D C00B H00E 107.9 . . ?
C006 C00C C00H 108.4(2) . . ?
C006 C00C H00F 110.0 . . ?
C00H C00C H00F 110.0 . . ?
C006 C00C H00G 110.0 . . ?
C00H C00C H00G 110.0 . . ?
H00F C00C H00G 108.4 . . ?
C00F C00D C007 121.0(3) . . ?
C00F C00D H00H 119.5 . . ?
C007 C00D H00H 119.5 . . ?
C00F C00E C005 117.9(2) . . ?
C00F C00E H00I 121.0 . . ?
C005 C00E H00I 121.0 . . ?
C00D C00F C00E 121.1(2) . . ?
C00D C00F H00J 119.4 . . ?
C00E C00F H00J 119.4 . . ?
C00I C00G C009 120.3(3) . . ?
C00I C00G H00K 119.8 . . ?
C009 C00G H00K 119.8 . . ?
C00B C00H C00C 111.4(2) . . ?
C00B C00H H00L 109.4 . . ?
C00C C00H H00L 109.4 . . ?
C00B C00H H00M 109.4 . . ?
C00C C00H H00M 109.4 . . ?
H00L C00H H00M 108.0 . . ?
C00J C00I C00G 119.0(3) . . ?
C00J C00I H00N 120.5 . . ?
C00G C00I H00N 120.5 . . ?
C00I C00J C00A 120.8(3) . . ?
C00I C00J H00O 119.6 . . ?
C00A C00J H00O 119.6 . . ?
 
_refine_diff_density_max    0.154
_refine_diff_density_min   -0.142
_refine_diff_density_rms    0.036



