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_2108898
_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         'C12 H17 O2 Si, C8 H12 N'
_chemical_formula_sum            'C20 H29 N O2 Si'
_chemical_formula_weight         343.544
_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
_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                   6.8160(14)
_cell_length_b                   12.721(3)
_cell_length_c                   23.613(5)
_cell_measurement_reflns_used    16341
_cell_measurement_temperature    25
_cell_measurement_theta_max      12.865
_cell_measurement_theta_min      0.43
_cell_volume                     2047.4(8)
_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)'
_diffrn_ambient_temperature      25
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.9984
_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      -0.081752
_diffrn_orient_matrix_UB_12      0.027734
_diffrn_orient_matrix_UB_13      0.031661
_diffrn_orient_matrix_UB_21      0.104075
_diffrn_orient_matrix_UB_22      -0.020522
_diffrn_orient_matrix_UB_23      0.027544
_diffrn_orient_matrix_UB_31      0.062589
_diffrn_orient_matrix_UB_32      0.070351
_diffrn_orient_matrix_UB_33      -0.004446
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3567
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.9984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17267
_diffrn_reflns_point_group_measured_fraction_full 0.9911
_diffrn_reflns_point_group_measured_fraction_max 0.9893
_diffrn_reflns_theta_full        12.3580
_diffrn_reflns_theta_max         12.91
_diffrn_reflns_theta_min         0.87
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.035
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       block
_exptl_crystal_F_000             743.771
_refine_diff_density_max         0.3377
_refine_diff_density_min         -0.2038
_refine_diff_density_rms         0.0623
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.5(17)
_refine_ls_d_res_high            0.7986
_refine_ls_d_res_low             11.8065
_refine_ls_goodness_of_fit_ref   1.0695
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0695
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+1.1599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1854
_refine_ls_wR_factor_ref         0.2065
_reflns_Friedel_coverage         0.977
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              29
_reflns_limit_l_min              -29
_reflns_number_gt                2694
_reflns_number_total             4173
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            px5037sup1.cif
_cod_data_source_block           silaamin
_cod_original_cell_volume        2047.4(7)
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               2108898
_olex2_refinement_description
;
1. Others
 Sof(Si01)=Sof(H01)=Sof(C1a)=Sof(H1aa)=Sof(H1ab)=Sof(H1ac)=Sof(H00f)=Sof(H00g)=
 Sof(Ca)=Sof(Haa)=Sof(Hab)=Sof(Hac)=1-FVAR(1)
 Sof(Si)=Sof(H)=Sof(C)=Sof(Ha)=Sof(Hb)=Sof(Hc)=Sof(C1)=Sof(H1a)=Sof(H1b)=
 Sof(H1c)=Sof(H00d)=Sof(H00e)=FVAR(1)
 Uiso(H00f)=Uiso(H00g)=Uiso(H00d)=Uiso(H00e)=FVAR(2)
 Uiso(H01)=Uiso(H)=Uiso(H1a)=Uiso(H1b)=Uiso(H1c)=Uiso(H1aa)=Uiso(H1ab)=
 Uiso(H1ac)=FVAR(3)
 Uiso(Haa)=Uiso(Hab)=Uiso(Hac)=FVAR(4)
2.a Ternary CH refined with riding coordinates:
 Si01(H01), Si(H), C006(H006), C008(H008)
2.b Secondary CH2 refined with riding coordinates:
 C00E(H00f,H00g), C00E(H00d,H00e)
2.c Aromatic/amide H refined with riding coordinates:
 C00L(H00o), C00I(H00p), C00J(H00q), C00A(H00r), C00D(H00s), C00K(H00K),
 C00H(H00H), C00F(H00i), C00B(H00j)
2.d Fitted hexagon refined as free rotating group:
 C00L(C00I,C00J,C00A,C007,C00D), C00G(C00K,C00H,C009,C00F,C00B)
2.e Idealised Me refined as rotating group:
 C(Ha,Hb,Hc), C1(H1a,H1b,H1c), C1a(H1aa,H1ab,H1ac), C00C(H00a,H00b,H00c),
 C00M(H00t,H00u,H00v), Ca(Haa,Hab,Hac)
;
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108898