A Practical and Efficient Route to Heteraphanes: Synthesis of Structurally Simplified Analogues of Ansamycins
Reddy, R. Santhosh; Zheng, Shaojun; lagishetti, chandraiah; You, Hengyao; He, Yun; RSC Adv.  (2016) –; doi:10.1039/C6RA16247A

data_7225832
_publ_section_title
;
 A Practical and Efficient Route to Heteraphanes: Synthesis of
 Structurally Simplified Analogues of Ansamycins
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA16247A
_journal_year                    2016
_chemical_formula_moiety         'C31 H34 N2 O8 S, C O'
_chemical_formula_sum            'C32 H34 N2 O9 S'
_chemical_formula_weight         622.67
_chemical_name_systematic        SAN-15
_chemical_temperature_decomposition_gt 493.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.09.16 svn.r3215 for OlexSys, GUI svn.r5097)
;
_audit_update_record
;
2016-02-29 deposited with the CCDC.
2016-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.577(5)
_cell_angle_beta                 96.639(4)
_cell_angle_gamma                104.437(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3398(4)
_cell_length_b                   11.7932(7)
_cell_length_c                   16.6442(9)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.4410
_cell_measurement_theta_min      3.5380
_cell_volume                     1529.21(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean 16.0892
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12102
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.018
_diffrn_reflns_theta_min         3.455
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       Block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0779P)^2^+0.9346P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4652
_reflns_number_total             6935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra16247a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified 'more than' ('>') a certain temperature. The value '>493.15
decomposed' was changed to '493.15' - it should be numeric and
without a unit designator.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        1529.22(15)
_cod_database_code               7225832
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00X(H00a,H00b), C011(H01d,H01e), C012(H01f,H01g), C013(H01h,H01i)
2.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00L(H00L), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U),
 C00V(H00V), C00W(H00W)
2.c Idealised Me refined as rotating group:
 C00Y(H00c,H00d,H00e), C010(H01a,H01b,H01c), C014(H01j,H01k,H01l), C015(H01m,
 H01n,H01o), C017(H01p,H01q,H01r), C018(H01s,H01t,H01u)
;
_shelx_res_checksum              17834
_olex2_submission_special_instructions 'No special instructions were received'