Ibuprofen and sila-ibuprofen: polarization effects in the crystal and enzyme environments
Kleemiss, Florian; Puylaert, Pim; Duvinage, Daniel; Fugel, Malte; Sugimoto, Kunihisa; Beckmann, Jens; Grabowsky, Simon; Acta Crystallographica Section B 77 (2021) 892–905; doi:10.1107/S2052520621009379

data_2108897
_publ_section_title
;
 Ibuprofen and sila-ibuprofen: polarization effects in the crystal and
 enzyme environments
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              892
_journal_page_last               905
_journal_paper_doi               10.1107/S2052520621009379
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C13 H17 O2, C8 H12 N'
_chemical_formula_sum            'C21 H29 N O2'
_chemical_formula_weight         327.470
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-03
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.04.27 svn.r7e0b91c7 for OlexSys, GUI svn.r6014)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9130(12)
_cell_length_b                   15.305(3)
_cell_length_c                   22.257(4)
_cell_measurement_reflns_used    106986
_cell_measurement_temperature    25
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      0.46
_cell_volume                     2014.2(7)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction
'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      25
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9997
_diffrn_measurement_device_type
'SPring8 beamline BL02B1 fitted with a curved image plate'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_UB_11      0.074995
_diffrn_orient_matrix_UB_12      0.046775
_diffrn_orient_matrix_UB_13      0.024369
_diffrn_orient_matrix_UB_21      -0.151885
_diffrn_orient_matrix_UB_22      0.023368
_diffrn_orient_matrix_UB_23      0.011784
_diffrn_orient_matrix_UB_31      -0.00105
_diffrn_orient_matrix_UB_32      -0.039368
_diffrn_orient_matrix_UB_33      0.035949
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3567
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.9997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            87404
_diffrn_reflns_point_group_measured_fraction_full 0.9959
_diffrn_reflns_point_group_measured_fraction_max 0.9937
_diffrn_reflns_theta_full        12.3580
_diffrn_reflns_theta_max         14.76
_diffrn_reflns_theta_min         0.92
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.027
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       platelet
_exptl_crystal_F_000             711.744
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.4971
_refine_diff_density_min         -0.3144
_refine_diff_density_rms         0.0787
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -4(7)
_refine_ls_d_res_high            0.7000
_refine_ls_d_res_low             11.1285
_refine_ls_goodness_of_fit_ref   1.0354
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6129
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.0337
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+2.4386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.986
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              31
_reflns_limit_l_min              -31
_reflns_number_gt                5977
_reflns_number_total             6129
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            px5037sup1.cif
_cod_data_source_block           ibuamin
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               2108897
_olex2_refinement_description
;
1. Shared sites
{C3, C00B}
{C0, C004}
2. Restrained distances
 C2-H2b
 1.12 with sigma of 0.02
 H2a-C2
 1.12 with sigma of 0.02
 H1-C1
 1.12 with sigma of 0.02
 C2-H2c
 1.12 with sigma of 0.02
3. Restrained angles
 H2a-C2-H2c
 fixed at 108 with sigma of 0.02
 H2a-C2-H2b
 fixed at 108 with sigma of 0.02
 H2b-C2-H2c
 fixed at 108 with sigma of 0.02
 H2a-C2-C1
 fixed at 112 with sigma of 0.02
 C1-C2-H2b
 fixed at 112 with sigma of 0.02
 C1-C2-H2c
 fixed at 112 with sigma of 0.02
 C3-C1-H1
 fixed at 107 with sigma of 0.02
 C0-C1-H1
 fixed at 104 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C0) = Uanis(C004)
Uanis(C3) = Uanis(C00B)
5. Others
 Sof(C004)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(H2c)=Sof(C00B)=Sof(C1)=Sof(H1)=1-
 FVAR(1)
 Sof(H00L)=Sof(C00N)=Sof(H00f)=Sof(H00h)=Sof(H00k)=Sof(C0)=Sof(C3)=Sof(C00L)=
 FVAR(1)
 Uiso(H2a)=Uiso(H2b)=Uiso(H2c)=FVAR(2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108897