Non-covalent S⋯O interactions control conformation in a scaffold that disrupts islet amyloid polypeptide fibrillation
Peacock, Hayden; Luo, Jinghui; Yamashita, Tohru; Luccarelli, James; Thompson, Sam; Hamilton, Andrew D.; Chem. Sci. 7 (2016) 6435–; doi:10.1039/C6SC00756B

data_1543600
_publ_section_title
;
 Non-covalent S&#x22EF;O interactions control conformation in a scaffold
 that disrupts islet amyloid polypeptide fibrillation
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              6435
_journal_paper_doi               10.1039/C6SC00756B
_journal_volume                  7
_journal_year                    2016
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C23 H27 I1 N4 O5 S2'
_chemical_formula_sum            'C23 H27 I N4 O5 S2'
_chemical_formula_weight         630.53
_chemical_melting_point          ?
_chemical_name_systematic        24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-09-17
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2016-02-16 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1030(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.66860(10)
_cell_length_b                   35.1961(4)
_cell_length_c                   15.4447(2)
_cell_measurement_reflns_used    12155
_cell_measurement_temperature    100
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     5174.29(11)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       CCD
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87503
_diffrn_reflns_theta_full        25.203
_diffrn_reflns_theta_max         29.305
_diffrn_reflns_theta_min         1.716
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             2544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.0018958
_refine_ls_shift/su_mean         0.0000437
_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: 
 961. 0.141E+04 822. 295. 56.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0763
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0763
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              49
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                9627
_reflns_number_total             14386
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.40
_oxford_diffrn_Wilson_scale      0.66
_oxford_refine_ls_r_factor_ref   0.0525
_oxford_refine_ls_scale          1.2335(19)
_oxford_reflns_number_all        12148
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'X:\SIMS\User\MT9981-24-05-14\010 At 17:46 on'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) H   ( 233,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 263,X'S) H   ( 262,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) H   ( 283,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) 
RIDE C   ( 122,X'S) H   (1222,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) H   (1233,X'S) H   (1232,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) H   (1252,X'S) 
RIDE C   ( 126,X'S) H   (1261,X'S) H   (1262,X'S) H   (1263,X'S) 
RIDE C   ( 134,X'S) H   (1342,X'S) H   (1341,X'S) H   (1343,X'S) 
RIDE C   ( 133,X'S) H   (1332,X'S) H   (1331,X'S) H   (1333,X'S) 
RIDE C   ( 132,X'S) H   (1322,X'S) H   (1321,X'S) H   (1323,X'S) 
RIDE C   ( 128,X'S) H   (1282,X'S) H   (1281,X'S) H   (1283,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
_cod_data_source_file            c6sc00756b2.cif
_cod_data_source_block           24
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1543600.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C23 H27 I1 N4 O5 S2'
_cod_database_code               1543600