Crystal structure of ajacisine D monohydrate, C30H44N2O9
Li, Guo-Qiang; Xu, Qing-Peng; Zhao, Yi-Ting; Li, Yun-Yi; Li, Yao-Lan; Wang, Guo-Cai; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 527–529; doi:10.1515/ncrs-2018-0531

data_8105769
_publ_section_title
;
 Crystal structure of ajacisine D monohydrate, C30H44N2O9
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              527
_journal_page_last               529
_journal_paper_doi               10.1515/ncrs-2018-0531
_journal_volume                  234
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C30 H42 N2 O8, H2 O'
_chemical_formula_sum            'C30 H44 N2 O9'
_chemical_formula_weight         576.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           Olex2
_cell_angle_alpha                90
_cell_angle_beta                 90.903(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9827(3)
_cell_length_b                   12.6787(6)
_cell_length_c                   14.0183(9)
_cell_measurement_reflns_used    3599
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.4840
_cell_measurement_theta_min      3.8210
_cell_volume                     1418.62(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[1]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[1]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)[2]'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)[2]'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
  1 omega    2.00   28.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       25.8250   77.0000 -150.0000 26

  2 omega -104.00  -76.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.8563 -178.0000 -150.0000 28

  3 omega -104.00  -71.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.8563  178.0000  150.0000 33

  4 omega  -90.00   32.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.8563    0.0000  -30.0000 122

  5 omega   20.00   46.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       25.6688   57.0000  120.0000 26

  6 omega   43.00   84.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       25.6688 -154.0000  -17.0000 41

  7 omega   20.00   56.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       25.6688  -19.0000  -60.0000 36

  8 omega  -47.00  -22.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       25.6688  -19.0000  -60.0000 25

  9 omega   57.00   83.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       25.6688  178.0000  -90.0000 26

 10 omega  -92.00   -6.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7000  -57.0000 -120.0000 86

 11 omega -101.00  -40.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7000 -178.0000 -120.0000 61

 12 omega  -74.00  -35.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.7000 -178.0000  -30.0000 39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Gemini S ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0095159000
_diffrn_orient_matrix_UB_12      0.0033483000
_diffrn_orient_matrix_UB_13      0.0501240000
_diffrn_orient_matrix_UB_21      -0.0264123000
_diffrn_orient_matrix_UB_22      -0.0534047000
_diffrn_orient_matrix_UB_23      0.0010693000
_diffrn_orient_matrix_UB_31      0.0843241000
_diffrn_orient_matrix_UB_32      -0.0163320000
_diffrn_orient_matrix_UB_33      0.0068181000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19473
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.808
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1891 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.5(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         9362
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                6262
_reflns_number_total             9362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0531_suppl.cif
_cod_data_source_block           lgq_fyc-44
_cod_database_code               8105769
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.975
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Rotating group:
 N2(H2A,H2B)
2.b Ternary CH refined with riding coordinates:
 C1(H1A), C5(H5A), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16),
 C17(H17)
2.c Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3A,H3B), C12(H12A,H12B), C15(H15A,H15B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B)
2.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29)
2.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
2.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O4(H4), O5(H5)
;
_shelx_res_checksum              6411
_shelx_hkl_checksum              72453
_olex2_submission_special_instructions 'No special instructions were received'