Structures of New Alkaloids from Rain Forest Trees <i>Galbulimima belgraveana</i> and <i>Galbulimima baccata</i> in Papua New Guinea, Indonesia, and Northern Australia.
Lan, Ping; Herlt, Anthony J.; Willis, Anthony C.; Taylor, Walter C.; Mander, Lewis N.; ACS omega 3 (2018) 1912–1921; doi:10.1021/acsomega.7b02065

data_4516029
_publ_section_title
;
 Structures of New Alkaloids from Rain Forest Trees <i>Galbulimima
 belgraveana</i> and <i>Galbulimima baccata</i> in Papua New Guinea,
 Indonesia, and Northern Australia.
;
_journal_issue                   2
_journal_name_full               'ACS omega'
_journal_page_first              1912
_journal_page_last               1921
_journal_paper_doi               10.1021/acsomega.7b02065
_journal_volume                  3
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_compound_source        local
_chemical_formula_moiety         'C24 H33 N O5'
_chemical_formula_sum            'C24 H33 N O5'
_chemical_formula_weight         415.53
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-05-27
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2015-05-27 - Report on C24 H33 N O5
             by Anthony C. Willis
             for   Ping Lan and Lew Mander

2015-05-27 - passes checkcif tests with warnings  
;
_cell_angle_alpha                69.268(5)
_cell_angle_beta                 89.374(4)
_cell_angle_gamma                71.779(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3874(3)
_cell_length_b                   10.6644(6)
_cell_length_c                   13.5952(7)
_cell_measurement_reflns_used    7234
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     1073.44(10)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2015)'
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
;
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2015)'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Supernova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12807
_diffrn_reflns_theta_full        72.322
_diffrn_reflns_theta_max         72.322
_diffrn_reflns_theta_min         3.498
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb 9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.21
_refine_ls_abs_structure_details 'Flack (1983), 1186 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.0011935
_refine_ls_shift/su_mean         0.0002306
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.15P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1294
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1294
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -10
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                5307
_reflns_number_total             5411
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.73
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0470
_oxford_refine_ls_scale          8.9(3)
_oxford_reflns_number_all        5411
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'Z:\man1506SN\Tony_man1506SN_data At 16:34 on'
_cod_data_source_file            14.cif
_cod_data_source_block           man1506SN
_cod_original_sg_symbol_Hall     'P 1 '
_cod_original_sg_symbol_H-M      'P 1 '
_cod_database_code               4516029
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S H(221,X'S) H(521,X'S) 
CONT ENANTIO 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) H   (  63,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 462,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 542,X'S) 

RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) H   ( 573,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 0.82, .02 = O(22) TO H(221) 
DIST 0.82, .02 = O(52) TO H(521) 
ANGLE 108, 2 = C(21) TO O(22) TO H(221) 
ANGLE 108, 2 = C(51) TO O(52) TO H(521) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;