Clarithromycin monohydrate: a synchrotron X-ray powder study
Noguchi, Shuji; Fujiki, Sadahiro; Iwao, Yasunori; Miura, Keiko; Itai, Shigeru; Acta Crystallographica Section E 68 (2012) o667–o668; doi:10.1107/S1600536812005090

data_2233827
_publ_section_title
;
 Clarithromycin monohydrate: a synchrotron X-ray powder study
;
_journal_coeditor_code           HB6588
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o667
_journal_page_last               o668
_journal_paper_doi               10.1107/S1600536812005090
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C38 H69 N O13, H2 O'
_chemical_formula_moiety         'C38 H69 N O13, H2 O'
_chemical_formula_structural     'C38 H69 N O13, H2 O'
_chemical_formula_sum            'C38 H71 N O14'
_chemical_formula_weight         765.969
_chemical_name_common            clarithromycin
_chemical_name_systematic
;(3<i>R</i>,4<i>S</i>,5<i>S</i>,6<i>R</i>,7<i>R</i>,9<i>R</i>,
11<i>S</i>,12<i>R</i>,13<i>S</i>,14<i>S</i>)-
6-{[(2<i>S</i>,3<i>R</i>,4<i>S</i>,6<i>R</i>)-4-dimethylamino-
3-hydroxy-6-methyloxan-2-yl]oxy}-14-ethyl-12,13-dihydroxy-
4-{[(2<i>R</i>,4<i>S</i>,5<i>S</i>,6<i>S</i>)-5-hydroxy-4-methoxy-
4,6-dimethyloxan-2-yl]oxy}-7-methoxy-3,5,7,9,11,13-hexamethyl-1-
oxacyclotetradecane-2,10-dione
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6999(2)
_cell_length_b                   18.8817(2)
_cell_length_c                   15.0267(2)
_cell_measurement_temperature    298
_cell_volume                     4454.53(9)
_computing_cell_refinement
;
<i>EXPO2009</i> (Altomare <i>et al.</i>, 2009) and
<i>RIETAN-FP</i> (Izumi & Momma, 2007)
;
_computing_data_collection
'local software (Osaka <i>et al.</i>, 2010; Takata <i>et al.</i>, 2002)'
_computing_data_reduction        'local software (Takata <i>et al.</i>, 2002)'
_computing_molecular_graphics
'<i>CCP4MG</i> (McNicholas <i>et al.</i>, 2011)'
_computing_publication_material  '<i>publCIF</i> (Westrip, 2010)'
_computing_structure_refinement
;
<i>CCP4</i> (Collaborative Computational Project, Number 4,
1994) and
<i>RIETAN-FP</i> (Izumi & Momma, 2007)
;
_computing_structure_solution
;
<i>CCP4</i> (Collaborative Computational Project, Number 4,
1994)
;
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'BL-19B2 Debye--Scherrer camera'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.3000
_exptl_absorpt_coefficient_mu    0.412
_exptl_crystal_density_diffrn    1.1421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672.00
_pd_block_id                     cam-form4
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     powder
_pd_meas_2theta_range_inc        0.0100
_pd_meas_2theta_range_max        65.0000
_pd_meas_2theta_range_min        3.0000
_pd_meas_number_of_points        6201
_pd_meas_scan_method             fixed
_pd_prep_pressure                101
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.0100
_pd_proc_2theta_range_max        65.0000
_pd_proc_2theta_range_min        3.0000
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_prof_R_factor        0.03817
_pd_proc_ls_prof_wR_expected     0.01574
_pd_proc_ls_prof_wR_factor       0.05225
_pd_proc_wavelength              1.3000
_pd_spec_mounting                capilary
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              3.0
_pd_spec_size_equat              0.3
_pd_spec_size_thick              0.3
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.3196
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           sparse
_refine_ls_number_constraints    0
_refine_ls_number_parameters     188
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.07572
_refine_ls_shift/su_max          0.0111
_refine_ls_shift/su_mean         0.000889
_refine_ls_weighting_details     1/[Y~i~]
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            hb6588.cif
_cod_data_source_block           I
_cod_database_code               2233827