A tendril perversion in a helical oligomer: trapping and characterizing a mobile screw-sense reversal.
Tomsett, Michael; Maffucci, Irene; Le Bailly, Bryden A. F.; Byrne, Liam; Bijvoets, Stefan M.; Lizio, M. Giovanna; Raftery, James; Butts, Craig P.; Webb, Simon J.; Contini, Alessandro; Clayden, Jonathan; Chemical science 8 (2017) 3007–3018; doi:10.1039/c6sc05474a

data_1545163
_publ_section_title
;
 A tendril perversion in a helical oligomer: trapping and characterizing a
 mobile screw-sense reversal.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              3007
_journal_page_last               3018
_journal_paper_doi               10.1039/c6sc05474a
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C55 H93 N11 O11'
_chemical_formula_weight         1084.40
_space_group_IT_number           4
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Mon Dec 23 11:18:49 2013'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_audit_update_record
;
2016-11-23 deposited with the CCDC.
2017-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 89.215(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6336(3)
_cell_length_b                   14.6369(3)
_cell_length_c                   33.2755(7)
_cell_measurement_reflns_used    12610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.6974
_cell_measurement_theta_min      2.6538
_cell_volume                     6639.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
  1 omega   89.40  227.40   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.8669  194.2088 184

  2 phi    -23.42  155.98   0.7506   16.0000
omega____ theta____ kappa____ phi______ frames
 154.2097  111.0000   73.8669     -     239

  3 omega  117.55  235.30   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669  289.2094 157

  4 phi    139.21  318.70   0.7510    7.5000
omega____ theta____ kappa____ phi______ frames
 132.6590  -25.0000   73.8670     -     239

  5 phi    -15.46  150.43   0.7506   16.0000
omega____ theta____ kappa____ phi______ frames
 140.3894  100.0000   73.8669     -     221

  6 omega  153.08  227.33   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669   24.2094 99

  7 omega  169.46  269.21   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  169.2088 133

  8 omega  170.92  251.92   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   73.8669  219.2088 108

  9 phi     63.98  136.79   0.7506    7.5000
omega____ theta____ kappa____ phi______ frames
  49.7594  -69.5000   73.8669     -     97

 10 phi    222.84  328.68   0.7506    7.5000
omega____ theta____ kappa____ phi______ frames
 125.1694   75.0000   73.8669     -     141

 11 omega   94.25  170.75   0.7500   16.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   73.8669  184.2094 102

;
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.1079503000
_diffrn_orient_matrix_UB_12      0.0034407000
_diffrn_orient_matrix_UB_13      -0.0131319000
_diffrn_orient_matrix_UB_21      0.0310988000
_diffrn_orient_matrix_UB_22      -0.0296556000
_diffrn_orient_matrix_UB_23      -0.0426764000
_diffrn_orient_matrix_UB_31      -0.0128489000
_diffrn_orient_matrix_UB_32      -0.1009022000
_diffrn_orient_matrix_UB_33      0.0121952000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_av_sigmaI/netI    0.1264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35552
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         74.6974
_diffrn_reflns_theta_min         2.6538
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.570
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.252
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(5)
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         16990
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.383
_refine_ls_R_factor_all          0.1879
_refine_ls_R_factor_gt           0.1544
_refine_ls_shift/su_max          1.718
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3885
_refine_ls_wR_factor_ref         0.4276
_reflns_number_gt                11058
_reflns_number_total             16990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc05474a2.cif
_cod_data_source_block           s3941na
_cod_depositor_comments
;Adding full bibliography for 1545162--1545163.cif.

 Adding full bibliography for 1545162--1545163.cif.
;
_cod_database_code               1545163