Solid-state NMR analysis of a complex crystalline phase of ronacaleret hydrochloride.
Vogt, Frederick G.; Williams, Glenn R.; Strohmeier, Mark; Johnson, Matthew N.; Copley, Royston C. B.; The journal of physical chemistry. B 118 (2014) 10266–10284; doi:10.1021/jp505061j

data_1517407
_publ_section_title
;
 Solid-state NMR analysis of a complex crystalline phase of ronacaleret
 hydrochloride.
;
_journal_issue                   34
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              10266
_journal_page_last               10284
_journal_paper_doi               10.1021/jp505061j
_journal_volume                  118
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H32 F2 N O4 +, Cl -'
_chemical_formula_sum            'C25 H32 Cl F2 N O4'
_chemical_formula_weight         483.97
_chemical_name_systematic
;
3-{3-[((2R)-3-{[2-(2,3-Dihydro-1H-inden-2-yl)-1,1-dimethylethyl]amino}-2-
hydroxypropyl)oxy]-4,5-difluorophenyl}propanoic acid, hydrochloride salt
;
_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_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.889(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6490(13)
_cell_length_b                   7.6848(14)
_cell_length_c                   23.486(7)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    150(2)
_cell_volume                     2445.7(9)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33318
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         8482
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+1.6589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                6872
_reflns_number_total             8482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp505061j_si_002.cif
_cod_data_source_block           x4563a1
_cod_depositor_comments          'Adding full bibliography for 1517407.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1517407