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_1565178
_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_formula_moiety         'C42.64 H56.23 Cl3.11 N16 O5.46'
_chemical_formula_sum            'C42.64 H56.23 Cl3.11 N16 O5.46'
_chemical_formula_weight         990.44
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2021-01-22 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.150(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.00486(4)
_cell_length_b                   18.58877(3)
_cell_length_c                   23.79439(4)
_cell_measurement_reflns_used    4657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      3
_cell_volume                     5279.29(5)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_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_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
;
Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.114
_diffrn_reflns_av_unetI/netI     0.181
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31995
_diffrn_reflns_theta_full        41.627
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.023
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2082.261
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.69
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 1818 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.22(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.7645
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6744
_refine_ls_number_restraints     675
_refine_ls_R_factor_all          0.2533
_refine_ls_R_factor_gt           0.1864
_refine_ls_shift/su_max          0.0370659
_refine_ls_shift/su_mean         0.0040268
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.5199
_refine_ls_wR_factor_gt          0.4695
_refine_ls_wR_factor_ref         0.4983
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                3801
_reflns_number_total             9165
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.11
_oxford_diffrn_Wilson_scale      0.96
_oxford_refine_ls_r_factor_ref   0.2252
_oxford_refine_ls_scale          0.624(3)
_oxford_reflns_number_all        9165
_cod_data_source_file            d1sc05021d2.cif
_cod_data_source_block           I_CCDC3
_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_cell_volume        5279.29(6)
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               1565178
_diffrn_radiation_collimation_monochromator 'Varimax focusing mirrors'
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  0.19(5)
_oxford_bijvoet_difference       0.22(4)