Understanding the structure details when drying hydrate crystals of pharmaceuticals ‒ interpretations from diffuse scattering and inter-modulation satellites of a partially dehydrated crystal
Chan, E. J.; Gao, Q.; Dabros, M.; Acta Crystallographica Section B 70 (2014) 555–567; doi:10.1107/S2052520614005125

data_2105818
_publ_section_title
;
 Understanding the structure details when drying hydrate crystals of
 pharmaceuticals -- interpretations from diffuse scattering and
 inter-modulation satellites of a partially dehydrated crystal
;
_journal_coeditor_code           WF5109
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              555
_journal_page_last               567
_journal_paper_doi               10.1107/S2052520614005125
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety
'C28 H29 F2 N6 O3 1+,0.5(O4 S1 2-),1.5(H2 O1)'
_chemical_formula_sum            'C28 H32 F2 N6 O6.5 S0.5'
_chemical_formula_weight         610.63
_chemical_name_systematic
;
 BMS-927711-0.5H2SO4 H1.5-1 sesquihydrate CGRP
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                   10.9169(9)
_cell_length_b                   33.039(3)
_cell_length_c                   7.9038(6)
_cell_measurement_reflns_used    7294
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      53.95
_cell_measurement_theta_min      2.67
_cell_volume                     2850.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18471
_diffrn_reflns_theta_full        55.05
_diffrn_reflns_theta_max         55.05
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.183
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0560P)^2^+1.0338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                3235
_reflns_number_total             3509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            wf5109sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2105818.cif.'
_cod_original_sg_symbol_Hall     P_2_2ab
_cod_original_sg_symbol_H-M      'P2(1)2(1)2 '
_cod_database_code               2105818