Cyclobuxophyllinine M, an alkaloid from <i>Buxus microphylla</i>
Hai-Feng Liu; Xiao-Qing Wu; Yan-Bing Duan; Min Ji; Acta Crystallographica Section E 63 (2007) o2194–o2195; doi:10.1107/S160053680701495X

data_2213577
_publ_section_title
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 Cyclobuxophyllinine M, an alkaloid from <i>Buxus microphylla</i>
;
_journal_coeditor_code           SK3099
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2194
_journal_page_last               o2195
_journal_paper_doi               10.1107/S160053680701495X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C25 H39 N O'
_chemical_formula_moiety         'C25 H39 N O'
_chemical_formula_sum            'C25 H39 N O'
_chemical_formula_weight         369.57
_chemical_melting_point          434.5(5)
_chemical_name_common            'Cyclobuxophyllinine M'
_chemical_name_systematic
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17-ethylidene-4,4,13,14-tetramethyl-3-
methylaminododecahydrocyclopropa[9,10]cyclopenta[<i>a</i>]phenanthren-16-one
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1102(13)
_cell_length_b                   11.054(2)
_cell_length_c                   27.294(5)
_cell_measurement_reflns_used    7398
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.2
_cell_volume                     2145.2(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2000)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20717
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+1.5605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                2128
_reflns_number_total             2269
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3099.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '434-435' was changed to '434.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '434-435' was changed to '434.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2213577
_cod_database_fobs_code          2213577