Bioactive Compounds from the Roots of Strophioblachia fimbricalyx.
Seephonkai, Prapairat; Pyne, Stephen G.; Willis, Anthony C.; Lie, Wilford; Journal of natural products 76 (2013) 1358–1364; doi:10.1021/np400268d

data_1512154
_publ_section_title
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 Bioactive Compounds from the Roots of Strophioblachia fimbricalyx.
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_journal_issue                   7
_journal_name_full               'Journal of natural products'
_journal_page_first              1358
_journal_page_last               1364
_journal_paper_doi               10.1021/np400268d
_journal_volume                  76
_journal_year                    2013
_chemical_compound_source        ' from U of Wollongong '
_chemical_formula_moiety         '2(C37 H36 O8), 3(C H Cl3)'
_chemical_formula_sum            'C77 H75 Cl9 O16'
_chemical_formula_weight         1575.51
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             12-10-12
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record
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2012-10-12 - Report C77 H75 Cl9 O16
             by Anthony C. Willis
             for Steve Pyne

2012-10-15 - pass checkcif tests with warnings  
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_cell_angle_alpha                90
_cell_angle_beta                 103.6646(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7937(8)
_cell_length_b                   7.7597(2)
_cell_length_c                   45.2891(18)
_cell_measurement_reflns_used    82074
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     7442.2(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
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ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
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_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    Superflip
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.163
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            60916
_diffrn_reflns_theta_full        22.496
_diffrn_reflns_theta_max         22.496
_diffrn_reflns_theta_min         2.625
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.61
_refine_diff_density_min         -1.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         9710
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.2459
_refine_ls_R_factor_gt           0.0859
_refine_ls_shift/su_max          0.0317339
_refine_ls_shift/su_mean         0.0021871
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
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 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.65 1.15 0.178 
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1720
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1720
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              48
_reflns_limit_l_min              0
_reflns_number_gt                3567
_reflns_number_total             9710
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.14
_oxford_diffrn_Wilson_scale      887.14
_oxford_refine_ls_r_factor_ref   0.2459
_oxford_refine_ls_scale          0.051536(9)
_oxford_reflns_number_all        9710
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '10111457 pyn1209 45'
_cod_data_source_file            np400268d_si_001.cif
_cod_data_source_block           Cmpd2
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_database_code               1512154
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, C(1,U'S) UNTIL CL(122) 
CONT C(130,U'S) UNTIL CL(134) CL(133,OCC) CL(134,OCC) 
EQUIV CL(133,OCC) CL(134,OCC) 
WEIGHT -1 CL(134,OCC) 
RIDE O(39,X'S) H(391,X'S) 
RIDE O(89,X'S) H(891,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) H   ( 403,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) H   ( 443,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) H   ( 822,X'S) H   ( 823,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) H   ( 833,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) H   ( 852,X'S) H   ( 853,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) H   ( 872,X'S) H   ( 873,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) H   ( 882,X'S) H   ( 883,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) H   ( 902,X'S) H   ( 903,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) H   ( 912,X'S) H   ( 913,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) H   ( 942,X'S) H   ( 943,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) H   ( 952,X'S) H   ( 953,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) 
RIDE C(130,X'S) H(1301,X'S) H(1302,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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DIST 1.70, .02 =  C(130) TO CL(131), C(130) TO CL(132) 
DIST 1.70, .02 =  C(130) TO CL(133), C(130) TO CL(134) 
ANGLE 113, 2. = CL(131) TO C(130) TO CL(132) 
ANGLE 113, 2. =  CL(131) TO C(130) TO CL(133), CL(132) TO C(130) TO CL(133) 
ANGLE 113, 2. =  CL(131) TO C(130) TO CL(134), CL(132) TO C(130) TO CL(134) 
DIST 2.85, .02 =  CL(131) TO CL(132) 
DIST 2.85, .02 =  CL(131) TO CL(133), CL(132) TO CL(133) 
DIST 2.85, .02 =  CL(131) TO CL(134), CL(132) TO CL(134) 
REM 
VIBR 0.0, 0.01 = C(130) TO CL(131), C(130) TO CL(132) 
CONT             C(130) TO CL(133), C(130) TO CL(134) 
VIBR 0.0, 0.01 = CL(131) TO CL(132) 
VIBR 0.0, 0.01 = CL(131) TO CL(133), CL(132) TO CL(133) 
VIBR 0.0, 0.01 = CL(131) TO CL(134), CL(132) TO CL(134) 
REM 
U(IJ) 0.0, .02 = CL(131) TO CL(133,-2,1,2,0,1) 
U(IJ) 0.0, .02 = CL(132) TO CL(134,-2,1,2,0,1) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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