Synthetic studies towards the Lycopodium alkaloid paniculatine
Lei, Shenghui; RSC Advances 3 (2013) 11014–; doi:10.1039/c3ra41467a

data_7239047
_publ_section_title
;
 Synthetic studies towards the Lycopodium alkaloid paniculatine
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              11014
_journal_paper_doi               10.1039/c3ra41467a
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'Cl, C17 H24 N O2, H2 O'
_chemical_formula_sum            'C17 H26 Cl N O3'
_chemical_formula_weight         327.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-09
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.010(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5230(3)
_cell_length_b                   9.6410(2)
_cell_length_c                   14.1520(4)
_cell_measurement_reflns_used    5395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.1209
_cell_measurement_theta_min      3.1900
_cell_volume                     1671.23(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 10.4015
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
1 omega -10.00 45.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 40.7390 -38.0000 60.0000 55
2 omega -3.00 61.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 40.7390 -99.0000 -120.0000 64
3 omega -20.00 64.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 40.7390 -38.0000 -90.0000 84
4 omega 20.00 109.00 1.0000 2.5000
omega____ theta____ kappa____ phi______ frames
- 40.7390 57.0000 30.0000 89
5 omega 78.00 132.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -92.0000 -120.0000 54
6 omega 7.00 67.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -91.0000 72.0000 60
7 omega 18.00 68.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -91.0000 -7.0000 50
8 omega 68.00 121.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -64.0000 142.0000 53
9 omega 11.00 55.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -92.0000 -120.0000 44
10 omega 79.00 154.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 77.0000 90.0000 75
11 omega 18.00 60.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -64.0000 142.0000 42
12 omega 65.00 129.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 45.0000 -180.0000 64
13 omega 25.00 67.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -45.0000 150.0000 42
14 omega 86.00 130.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -91.0000 72.0000 44
15 omega 73.00 131.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -91.0000 -7.0000 58
16 omega 22.00 77.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -45.0000 60.0000 55
17 omega 73.00 157.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 125.0000 150.0000 84
18 omega 32.00 164.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 15.0000 30.0000 132
19 omega 78.00 105.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 125.0000 30.0000 27
20 omega 125.00 166.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 125.0000 30.0000 41
21 omega 96.00 126.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -91.0000 133.0000 30
22 omega 55.00 81.00 1.0000 7.5000
omega____ theta____ kappa____ phi______ frames
- 92.5000 -91.0000 133.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0003064000
_diffrn_orient_matrix_UB_12      0.1130391000
_diffrn_orient_matrix_UB_13      -0.0769678000
_diffrn_orient_matrix_UB_21      0.0037149000
_diffrn_orient_matrix_UB_22      -0.1129253000
_diffrn_orient_matrix_UB_23      -0.0763463000
_diffrn_orient_matrix_UB_31      -0.1256740000
_diffrn_orient_matrix_UB_32      -0.0036466000
_diffrn_orient_matrix_UB_33      -0.0252554000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13385
_diffrn_reflns_theta_full        67.23
_diffrn_reflns_theta_max         67.23
_diffrn_reflns_theta_min         3.61
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.3536
_exptl_crystal_size_mid          0.1447
_exptl_crystal_size_min          0.0949
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                2328
_reflns_number_total             2934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41467a.txt
_cod_data_source_block           exp_462
_cod_original_cell_volume        1671.24(8)
_cod_database_code               7239047
_chemical_oxdiff_formula         C17H26O3N1Cl1
_chemical_oxdiff_usercomment     qiufayang_leishenghui_20120605
_reflns_odcompleteness_completeness 98.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97