Crystal structure of 14-((1-(benzyloxycarbonyl-amino)-2-methylpropan-2-yl)sulfanyl)acetate Mutilin, C34H49NO6S
Shang, Ruofeng; Yi, Yunpeng; Liang, Jianping; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 465–467; doi:10.1515/ncrs-2015-0142

data_8106909
_publ_section_title
;
 Crystal structure of
 14-((1-(benzyloxycarbonyl-amino)-2-methylpropan-2-yl)sulfanyl)acetate
 Mutilin, C34H49NO6S
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              465
_journal_page_last               467
_journal_paper_doi               10.1515/ncrs-2015-0142
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C34 H49 N O6 S'
_chemical_formula_sum            'C34 H49 N O6 S'
_chemical_formula_weight         599.80
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.210(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7112(8)
_cell_length_b                   10.0135(5)
_cell_length_c                   14.6411(10)
_cell_measurement_reflns_used    1246
_cell_measurement_temperature    293.33(10)
_cell_measurement_theta_max      19.8250
_cell_measurement_theta_min      3.9970
_cell_volume                     1664.43(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.33(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -10.00   23.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000  150.0000 22

  2 omega  -39.00   63.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -19.0000  -60.0000 68

  3 omega   -5.00   83.50   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   38.0000  -30.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0400625000
_diffrn_orient_matrix_UB_12      -0.0001141000
_diffrn_orient_matrix_UB_13      -0.0450595000
_diffrn_orient_matrix_UB_21      0.0476559000
_diffrn_orient_matrix_UB_22      0.0071359000
_diffrn_orient_matrix_UB_23      -0.0215638000
_diffrn_orient_matrix_UB_31      0.0049203000
_diffrn_orient_matrix_UB_32      -0.0704742000
_diffrn_orient_matrix_UB_33      -0.0021032000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.1106
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6782
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_min         3.269
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 739 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5443
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0439P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.569
_reflns_Friedel_fraction_full    0.656
_reflns_Friedel_fraction_max     0.641
_reflns_number_gt                2861
_reflns_number_total             5443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2015-0142_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1664.43(18)
_cod_database_code               8106909
_reflns_odcompleteness_completeness 99.70
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A), C4(H4), C5(H5), C8(H8), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C0AA(H0AA,H0AB), C10(H10A,H10B), C11(H11A,H11B), C16(H16A,
 H16B), C17(H17A,H17B), C25(H25A,H25B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C13(H13), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
2.d X=CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C)
2.f Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              67061
_shelx_hkl_checksum              40520
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-06-29
_olex2_submission_special_instructions 'No special instructions were received'