Clarithromycin form I determined by synchrotron X-ray powder diffraction
Noguchi, Shuji; Miura, Keiko; Fujiki, Sadahiro; Iwao, Yasunori; Itai, Shigeru; Acta Crystallographica Section C 68 (2012) o41–o44; doi:10.1107/S0108270111054230

data_2018369
_publ_section_title
;
 Clarithromycin form I determined by synchrotron X-ray powder diffraction
;
_journal_coeditor_code           CU3008
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o41
_journal_page_last               o44
_journal_paper_doi               10.1107/S0108270111054230
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C38 H69 N1 O13'
_chemical_formula_moiety         'C38 H69 N1 O13'
_chemical_formula_sum            'C38 H69 N O13'
_chemical_formula_weight         748.0
_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_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   14.4531(4)
_cell_length_b                   34.6885(8)
_cell_length_c                   8.7114(2)
_cell_measurement_temperature    300
_cell_volume                     4367.52(19)
_computing_cell_refinement
;
EXPO2009 (Altomare, Camalli <i>et al.</i>, 2009) and RIETAN-FP (Izumi
& Momma, 2007)
;
_computing_data_collection       'local software (Takata <i>et al.</i>, 2002)'
_computing_data_reduction        'local software (Takata <i>et al.</i>, 2002)'
_computing_molecular_graphics    'CCP4MG (McNicholas <i>et al.</i>, 2011)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'RIETAN-FP (Izumi & Momma, 2007)'
_computing_structure_solution
'CCP4 (Collaborative Computational Project, Number 4, 1994)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Debye-Scherrer camera'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.3000
_exptl_absorpt_coefficient_mu    0.42
_exptl_crystal_density_diffrn    1.138
_pd_char_colour                  white
_pd_char_particle_morphology     powder
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        65.00
_pd_meas_2theta_range_min        3.00
_pd_meas_number_of_points        6201
_pd_meas_scan_method             fixed
_pd_prep_pressure                101
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        65.00
_pd_proc_2theta_range_min        3.00
_pd_proc_ls_background_function  'Legendre polynomial'
_pd_proc_ls_pref_orient_corr
;
March-Dollase preferential orientation correction
plane (0 1 0)
G factor 1.185(2)
;
_pd_proc_ls_profile_function     'split psudo-Voigt function'
_pd_proc_ls_prof_R_factor        0.03818
_pd_proc_ls_prof_wR_expected     0.01530
_pd_proc_ls_prof_wR_factor       0.05665
_pd_proc_wavelength              1.3000
_pd_spec_mounting                capillary
_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         0.267
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.703
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           sparse
_refine_ls_number_constraints    0
_refine_ls_number_parameters     185
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.04213
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.0003
_refine_ls_weighting_details     1/[Y~i~]
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            cu3008.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C38 H69 N1 O13'
_cod_database_code               2018369