Structure–property relations of a unique and systematic dataset of 19 isostructural multicomponent apremilast forms
Jirát, Jan; Babor, Martin; Ridvan, Luděk; Skořepová, Eliška; Dušek, Michal; Šoóš, Miroslav; IUCrJ 9 (2022) –; doi:10.1107/S2052252522005577

data_1567128
_publ_section_title
;
 Structure--property relations of a unique and systematic dataset of 19
 isostructural multicomponent apremilast forms
;
_journal_coeditor_code           ED5027
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252522005577
_journal_volume                  9
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H30.50 N2 O7 S1'
_chemical_formula_sum            'C26 H30.5 N2 O7 S'
_chemical_formula_weight         515.10
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.18500(10)
_cell_length_b                   13.18500(10)
_cell_length_c                   28.59300(10)
_cell_measurement_reflns_used    65234
_cell_measurement_temperature    120
_cell_measurement_theta_max      68
_cell_measurement_theta_min      4
_cell_volume                     4970.73(6)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            97817
_diffrn_reflns_theta_full        67.660
_diffrn_reflns_theta_max         67.660
_diffrn_reflns_theta_min         3.692
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.78
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 1844 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   -0.001(2)
_refine_ls_extinction_coef       46(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4498
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.0012206
_refine_ls_shift/su_mean         0.0000466
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 971. 0.155E+04 843. 281. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0598
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0598
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                4440
_reflns_number_total             4498
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.87
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0277
_oxford_refine_ls_scale          3.57(3)
_oxford_reflns_number_all        4498
_cod_data_source_file            ed5027.cif
_cod_data_source_block           Apremilast_paraxylene
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4970.73(8)
_cod_original_sg_symbol_H-M      'P 41 21 2 '
_cod_original_formula_sum        'C26 H30.50 N2 O7 S1'
_cod_database_code               1567128
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  -0.0000(7)
_oxford_bijvoet_difference       -0.001(2)
_oxford_refined_flack_x          0.004(16)