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_4516028
_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 ad
_chemical_compound_source        local
_chemical_formula_moiety         'C21 H31 N O2, 0.512(H2 O), 0.488(C H4 O)'
_chemical_formula_sum            'C21.488 H33.976 N O3'
_chemical_formula_weight         354.35
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             15-05-12
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2015-05-12 - Report on C21.488 H33.976 N O3
             by Anthony C. Willis
             for   Ping Lan and Lew Mander

2015-05-12 - passes checkcif tests with warnings  
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8673(2)
_cell_length_b                   9.5188(2)
_cell_length_c                   26.3409(5)
_cell_measurement_reflns_used    11379
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     1972.60(8)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.024
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23772
_diffrn_reflns_theta_full        72.283
_diffrn_reflns_theta_max         72.283
_diffrn_reflns_theta_min         4.940
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.82
_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            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             775.634
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.11
_refine_diff_density_min         -0.13
_refine_ls_abs_structure_details 'Flack (1983), 1637 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.04(18)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.0030591
_refine_ls_shift/su_mean         0.0003137
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 0.37P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0785
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0785
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                3769
_reflns_number_total             3889
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.03
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0324
_oxford_refine_ls_scale          7.96(17)
_oxford_reflns_number_all        3889
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title
'Z:\man1501SN\Tony_man1501SN_data At 17:44 on'
_cod_data_source_file            17.cif
_cod_data_source_block           man1501SN
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4516028
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
CONT C(25,OCC) UNTIL  O(27) H(111,X'S) 
EQUIV C(25,OCC) UNTIL  O(27) 
WEIGHT -1 O(27,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) H   ( 133,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) H   ( 172,X'S) 
RIDE C   (  18,X'S) H   ( 181,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   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C(25,X'S) H(251,X'S) H(252,X'S) H(253,X'S) 
RIDE O(26,X'S) H(261,X'S) 
RIDE O(27,X'S) H(271,X'S) H(272,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
U(IJ) 0.0, .001 = C(25) TO O(26) 
U(IJ) 0.0, .001 = C(25) TO O(27) 
U(IJ) 0.0, .001 = O(26) TO O(27) 
DIST 1.41, .01 = C(25) TO O(26) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;