Acid-mediated topological control in a functionalized foldamer
Knipe, Peter C.; Thompson, Sam; Hamilton, Andrew D.; Chemical Communications (Cambridge, United Kingdom) 52 (2016) 6521–6524; doi:10.1039/c6cc01496h

data_7119100
_publ_section_title
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 Acid-mediated topological control in a functionalized foldamer
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   39
_journal_name_full
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 Chemical Communications (Cambridge, United Kingdom)
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_journal_page_first              6521
_journal_page_last               6524
_journal_paper_doi               10.1039/c6cc01496h
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C21 H17 Br1 N4 O5 S1'
_chemical_formula_sum            'C21 H17 Br N4 O5 S'
_chemical_formula_weight         517.36
_chemical_melting_point          ?
_chemical_name_systematic        5
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-08
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2016-02-16 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.337(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.8020(11)
_cell_length_b                   5.04894(13)
_cell_length_c                   10.7810(3)
_cell_measurement_reflns_used    4336
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      6
_cell_volume                     2106.05(10)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20409
_diffrn_reflns_theta_full        72.562
_diffrn_reflns_theta_max         76.769
_diffrn_reflns_theta_min         4.112
_diffrn_standards_decay_%        .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.966
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details 'Flack (1983), 1868 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.013(10)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9493
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4322
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.0005642
_refine_ls_shift/su_mean         0.0000530
_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: 
 0.293E+04 0.508E+04 0.330E+04 0.154E+04 408. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0792
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0792
_reflns_limit_h_max              48
_reflns_limit_h_min              -48
_reflns_limit_k_max              6
_reflns_limit_k_min              -6
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                4281
_reflns_number_total             4336
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.54
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0304
_oxford_refine_ls_scale          3.91(4)
_oxford_reflns_number_all        4322
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '013pck15 in C2'
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            c6cc01496h5.cif
_cod_data_source_block           5
_cod_depositor_comments
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The following automatic conversions were performed:

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

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

Automatic conversion script
Id: cif_fix_values 4624 2016-04-14 12:54:50Z antanas 
;
_cod_original_sg_symbol_H-M      'C 1 2 1 '
_cod_original_formula_sum        'C21 H17 Br1 N4 O5 S1'
_cod_database_code               7119100