[1‒9-NαC]-Linusorb B3 (Cyclolinopeptide A) dimethyl sulfoxide monosolvate
Purdy, Sarah Kendra; Spasyuk, Denis; Chitanda, Jackson Mulenga; Reaney, Martin J. T.; IUCrData 5 (2020) x200318–; doi:10.1107/S2414314620003181

data_1557611
_publ_section_title
;
 [1--9-N\aC]-Linusorb B3 (Cyclolinopeptide A) dimethyl sulfoxide
 monosolvate
;
_journal_coeditor_code           LH4052
_journal_issue                   3
_journal_name_full               IUCrData
_journal_page_first              x200318
_journal_paper_doi               10.1107/S2414314620003181
_journal_volume                  5
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C57 H84 N9 O9, C2 H6 O S'
_chemical_formula_moiety         'C57 H84 N9 O9, C2 H6 O S'
_chemical_formula_sum            'C59 H90 N9 O10 S'
_chemical_formula_weight         1117.45
_chemical_name_common
;
[1--9-N\aC]-Linusorb B3 (Cyclolinopeptide A) dimethyl sulfoxide monosolvate
;
_chemical_name_systematic
'24,27-Dibenzyl-15,18-bis(butan-2-yl)-12,21-bis(2-methylpropyl)-9-(propan-2-yl)-1,7,10,13,16,19,22,25,28-nonaazatricyclo[28.3.0.0^3,7^]tritriacontane-2,8,11,14,17,20,23,26,29-nonone dimethyl sulfoxide monosolvate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.942(2)
_cell_length_b                   22.986(5)
_cell_length_c                   26.512(5)
_cell_measurement_reflns_used    17346
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.477
_cell_measurement_theta_min      1.136
_cell_volume                     6059(2)
_computing_cell_refinement
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_data_collection
;
<i>MxDC</i> (Fodje, 2012)
;
_computing_data_reduction
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_molecular_graphics
;
<i>ShelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_publication_material
;
<i>LinXTL</i> (Spasyuk, 2009) and
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008b)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rayonix MX300HE CCD area detector'
_diffrn_measurement_method       '\k and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68882
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            83438
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.136
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.4148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.295
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4488 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       0.0137(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11739
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+1.3012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                10684
_reflns_number_total             11739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh4052sup1.cif
_cod_data_source_block           I
_cod_database_code               1557611
_shelx_hkl_checksum              3880
_shelx_res_checksum              62106
_cod_database_fobs_code 1557611