Formation and Characterization of Crystals Containing a Pleuromutilin Derivative, Succinic Acid and Water
Clawson, Jacalyn S.; Vogt, Frederick G.; Brum, Jeffrey; Sisko, Joseph; Patience, Daniel B.; Dai, Wenning; Sharpe, Sonja; Jones, Alan D.; Pham, Tran N.; Johnson, Matthew N.; Copley, Royston C. P.; Crystal Growth & Design 8 (2008) 4120–; doi:10.1021/cg8005713

data_4503831
_publ_section_title
;
 Formation and Characterization of Crystals Containing a Pleuromutilin
 Derivative, Succinic Acid and Water
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4120
_journal_paper_doi               10.1021/cg8005713
_journal_volume                  8
_journal_year                    2008
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C28 H45 N2 O6 +, C4 H5 O4 -'
_chemical_formula_sum            'C32 H50 N2 O10'
_chemical_formula_weight         622.74
_chemical_name_common            'I (disordered succinic acid and solvent)'
_chemical_name_systematic
;
 Iminodicarboxylic acid trans-4-aminocyclohexyl mutilin-14 ester (salt)
;
_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
_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                   9.5171(11)
_cell_length_b                   16.7926(19)
_cell_length_c                   24.166(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3862.1(8)
_computing_cell_refinement       'SMART V5.054 [NT] (Bruker, 2000)'
_computing_data_collection       'SMART V5.054 [NT] (Bruker, 2000)'
_computing_data_reduction        'SAINT+ V6.22 [NT] (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 [NT] (Bruker, 2001)'
_computing_publication_material  'SHELXTL V6.10 [NT] (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 [NT] (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 [NT] (Bruker, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART 1K'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    '0.8 mm double-pinhole'
_diffrn_radiation_monochromator  'graphite - parallel geometry'
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21469
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0009(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0995P)^2^+1.8309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                2698
_reflns_number_total             3152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg8005713_si_003.cif
_cod_data_source_block           x4279a3
_cod_database_code               4503831