Specific Interactions between Rifamycin Antibiotics and Water Influencing Ability To Overcome Natural Cell Barriers and the Range of Antibacterial Potency.
Pyta, Krystian; Janas, Anna; Skrzypczak, Natalia; Schilf, Wojciech; Wicher, Barbara; Gdaniec, Maria; Bartl, Franz; Przybylski, Piotr; ACS infectious diseases 5 (2019) 1754–1763; doi:10.1021/acsinfecdis.9b00176

data_4515176
_publ_section_title
;
 Specific Interactions between Rifamycin Antibiotics and Water Influencing
 Ability To Overcome Natural Cell Barriers and the Range of Antibacterial
 Potency.
;
_journal_issue                   10
_journal_name_full               'ACS infectious diseases'
_journal_page_first              1754
_journal_page_last               1763
_journal_paper_doi               10.1021/acsinfecdis.9b00176
_journal_volume                  5
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C43 H58 N4 O12, 3(C H4 O)'
_chemical_formula_sum            'C46 H70 N4 O15'
_chemical_formula_weight         919.06
_chemical_name_common            'rifampicin methanol trisolvate'
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1242(6)
_cell_length_b                   13.9473(6)
_cell_length_c                   35.3927(17)
_cell_measurement_reflns_used    4434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      1.85
_cell_volume                     4997.6(4)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2002)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis CCD (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Kuma KM4CCD \k geometry'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_unetI/netI     0.3448
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19796
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         4.102
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SCALE3 ABSPACK scaling algorithm
(Oxford Diffraction, 2007) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 972 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8422
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.828
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0275P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.905
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                3174
_reflns_number_total             8422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            id9b00176_si_003.cif
_cod_data_source_block           rifampicin_methanol_trisolvate
_cod_database_code               4515176
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              62163
_shelx_hkl_checksum              4247