Isomorphism, Disorder, and Hydration in the Crystal Structures of Racemic and Single-Enantiomer Carvedilol Phosphate
Vogt, Frederick G.; Copley, Royston C. B.; Mueller, Ronald L.; Spoors, Grant P.; Cacchio, Thomas N.; Carlton, Robert A.; Katrincic, Lee M.; Kennady, James M.; Parsons, Simon; Chetina, Olga V.; Crystal Growth & Design 10 (2010) 2713–; doi:10.1021/cg100209v

data_4501668
_publ_section_title
;
 Isomorphism, Disorder, and Hydration in the Crystal Structures of Racemic
 and Single-Enantiomer Carvedilol Phosphate
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2713
_journal_paper_doi               10.1021/cg100209v
_journal_volume                  10
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H27 N2 O4 +, H2 O4 P -, 0.5 H2 O'
_chemical_formula_sum            'C24 H30 N2 O8.5 P'
_chemical_formula_weight         513.47
_chemical_name_systematic
;
 (2R)-1-(9H-Carbazol-4-yloxy)-3-[(2-{[2-(methyloxy)phenyl]oxy}ethyl)amino]-
 2-propanol, phosphoric acid salt, hemihydrate [ratio 1:1:0.5(H2O)]
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.1488(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.7679(6)
_cell_length_b                   12.2428(3)
_cell_length_c                   16.2786(4)
_cell_measurement_temperature    90(2)
_cell_volume                     5069.3(2)
_computing_cell_refinement       'SMART V5.604 [NT] (Bruker, 2000)'
_computing_data_collection       'SMART V5.604 [NT] (Bruker, 2000)'
_computing_data_reduction        'SAINT+ V6.45A [NT] (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL V6.10 UNIX (Bruker, 2001)'
_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      90(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24604
_diffrn_reflns_theta_full        73.26
_diffrn_reflns_theta_max         73.26
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  0.8537
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         9105
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+2.5150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                8951
_reflns_number_total             9105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100209v_si_002.cif
_cod_data_source_block           I-R
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C24 H30 N2 O8.50 P'
_cod_database_code               4501668