Tiamulin–hydrogen fumarate–methanol (1/1/1)
Xiao-Ji Cao; Cui-Rong Sun; Yuan-Jiang Pan; Acta Crystallographica Section E 60 (2004) o1546–o1548; doi:10.1107/S1600536804019713

data_2204135
_publ_section_title
;
 Tiamulin--hydrogen fumarate--methanol (1/1/1)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1546
_journal_page_last               o1548
_journal_paper_doi               10.1107/S1600536804019713
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C28 H48 N O4 S +, C4 H3 O4 -, C H4 O'
_chemical_formula_moiety         'C28 H48 N O4 S +, C4 H3 O4 -, C H4 O'
_chemical_formula_sum            'C33 H55 N O9 S'
_chemical_formula_weight         641.84
_chemical_name_systematic
;
6-ethenyldecahydro-5-hydroxy-4,6,9,10-tetramethyl-1-oxo-
3a,9-propano-3aH-cyclopentacycloocten-8-yl
[2-(diethylammonio)ethylsulfanyl]acetate (E)-3-carboxyprop-2-enoate methanol
solvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9350(10)
_cell_length_b                   10.0720(10)
_cell_length_c                   34.987(7)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.81
_cell_measurement_theta_min      3.37
_cell_volume                     3501.0(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Siemens, 1991)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            8625
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        5.38
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.9216
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XSCANS; Siemens, 1994)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.120
_refine_ls_abs_structure_details 'Flack (1983), 2981 Friedel pairs'
_refine_ls_abs_structure_Flack   0.03(8)
_refine_ls_extinction_coef       0.0069(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7293
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0444P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4560
_reflns_number_total             7293
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6411.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3501.0(8)
_cod_database_code               2204135
_cod_database_fobs_code          2204135