Chiral, Sequence-Definable Foldamer-Derived Macrocycles
Warnock, Toyah M. C.; Rajkumar, Sundaram; Fitzpatrick, Matthew; Serpell, Christopher J.; Dingwall, Paul; Knipe, Peter Clarke; Chemical Science  (2021) –; doi:10.1039/D1SC05021D

data_1565177
_publ_section_title
;
 Chiral, Sequence-Definable Foldamer-Derived Macrocycles
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05021D
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C21 H27 Cl N8 O2'
_chemical_formula_sum            'C21 H27 Cl N8 O2'
_chemical_formula_weight         458.9497
_chemical_name_systematic        'Dimer 2a'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2021-01-20 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0868(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.69330(10)
_cell_length_b                   9.01790(10)
_cell_length_c                   13.41980(10)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    100
_cell_measurement_theta_max      71
_cell_measurement_theta_min      6
_cell_volume                     1173.07(2)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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_pressure         100
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_unetI/netI     0.033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10892
_diffrn_reflns_theta_full        69.243
_diffrn_reflns_theta_max         71.384
_diffrn_reflns_theta_min         4.562
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.728
_exptl_absorpt_correction_T_max  0.42
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 1450 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.015(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.9544
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3842
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.0003449
_refine_ls_shift/su_mean         0.0000630
_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: 
 9.59 12.4 2.85 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0637
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0637
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              7
_reflns_limit_k_min              -10
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3806
_reflns_number_total             3858
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      0.24
_oxford_refine_ls_r_factor_ref   0.0342
_oxford_refine_ls_scale          0.8801(13)
_oxford_reflns_number_all        3842
_cod_data_source_file            d1sc05021d2.cif
_cod_data_source_block           I_CCDC2
_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_sg_symbol_H-M      'P 21 '
_cod_database_code               1565177
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  -0.001(5)
_oxford_bijvoet_difference       0.015(5)
_oxford_refined_flack_x          0.013(16)