Cyclolinopeptide B methanol trisolvate
Schatte, Gabriele; Labiuk, Shaunivan; Li, Bonnie; Burnett, Peta-Gaye; Reaney, Martin; Grochulski, Pawel; Fodje, Michel; Yang, Jian; Sammynaiken, Ramaswami; Acta Crystallographica Section E 68 (2012) o50–o51; doi:10.1107/S1600536811051488

data_2233239
_publ_section_title
;
 Cyclolinopeptide B methanol trisolvate
;
_journal_coeditor_code           LH5387
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o50
_journal_page_last               o51
_journal_paper_doi               10.1107/S1600536811051488
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C56 H83 N9 O9 S, 3C H4 O'
_chemical_formula_moiety         'C56 H83 N9 O9 S, 3(C H4 O)'
_chemical_formula_sum            'C59 H95 N9 O12 S'
_chemical_formula_weight         1154.50
_chemical_name_common
;
<i>cyclo</i>-(Met-Leu-Ile-Pro-Pro-Phe-Phe-Val-Ile)
;
_chemical_name_systematic
;
Cyclolinopeptide B methanol trisolvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0653(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.374(2)
_cell_length_b                   19.624(4)
_cell_length_c                   15.576(4)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      2.35
_cell_volume                     3122.1(12)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_data_collection
;
<i>MXDC</i>, Macromolecular Crystallography Data Collector (Canadian
Light Source, 2007)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>CAMERON</i> (Watkin <i>et al.</i>, 1993) and SHELXTL (Sheldrick,
2008)
;
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution
;
<i>SIR2004</i> (Burla <i>et al.</i>, 2005)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
300mm 16K Rayonix MX300 HE CCD detector with
an ACCEL MD2 microdiffractometer
;
_diffrn_measurement_method       'CCD rotation images, \w scans'
_diffrn_radiation_monochromator  'double crystal Si(111)'
_diffrn_radiation_source         'Beamline 08B1-1 at the CLS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68878
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            177237
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_correction_T_min  0.9849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.335
_refine_ls_abs_structure_details 'Flack (1983), 7080 Friedel pairs'
_refine_ls_abs_structure_Flack   0.09(7)
_refine_ls_extinction_coef       0.0195(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         15255
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.9515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                13940
_reflns_number_total             15255
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5387.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233239
_cod_database_fobs_code          2233239