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_4503830
_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         '2(C28 H45 N2 O6) +, (C4 H4 O4) 2-, 6(C H4 O)'
_chemical_formula_sum            'C66 H118 N4 O22'
_chemical_formula_weight         1319.64
_chemical_name_common            '0.5:1:6 succinic acid:I:methanol'
_chemical_name_systematic
;
 Iminodicarboxylic acid trans-4-aminocyclohexyl mutilin-14 ester, 
 succinic acid salt, methanol solvate (2:1:6)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.237(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3920(6)
_cell_length_b                   16.8501(11)
_cell_length_c                   23.7478(16)
_cell_measurement_temperature    150(2)
_cell_volume                     3758.2(4)
_computing_cell_refinement       'SMART V5.604 [NT] (Bruker, 2000)'
_computing_data_collection       'SMART V5.604 [NT] (Bruker, 2000)'
_computing_data_reduction        'SAINT+ V6.02A [NT] (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL V5.10 UNIX (Bruker, 1997)'
_computing_publication_material  'SHELXTL V6.10 UNIX (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 UNIX (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 UNIX (Bruker, 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker AXS SMART 6000'
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26441
_diffrn_reflns_theta_full        72.03
_diffrn_reflns_theta_max         72.03
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.7398
_exptl_absorpt_correction_T_min  0.6953
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         7381
_refine_ls_number_restraints     789
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1636P)^2^+2.3707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2213
_refine_ls_wR_factor_ref         0.2226
_reflns_number_gt                7214
_reflns_number_total             7381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg8005713_si_002.cif
_cod_data_source_block           x4279a2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4503830