Helicity adaptation within a quadruply stranded helicate by encapsulation.
Lin, Qi; Gao, Lei; Kauffmann, Brice; Zhang, Jiajia; Ma, Chunmiao; Luo, Dan; Gan, Quan; Chemical communications (Cambridge, England) 54 (2018) 13447–13450; doi:10.1039/c8cc07932c

data_7122553
_publ_section_title
;
 Helicity adaptation within a quadruply stranded helicate by
 encapsulation.
;
_journal_issue                   95
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13447
_journal_page_last               13450
_journal_paper_doi               10.1039/c8cc07932c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C128 H124 F4 N24 O16 Pd2'
_chemical_formula_sum            'C128 H124 F4 N24 O16 Pd2'
_chemical_formula_weight         2543.30
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-25 deposited with the CCDC.
2018-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.9268(6)
_cell_length_b                   18.9268(6)
_cell_length_c                   24.7717(9)
_cell_measurement_reflns_used    4581
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      71.3930
_cell_measurement_theta_min      5.5070
_cell_volume                     8873.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     38.00  63.00   0.50  115.00    --   94.60 -65.00-175.00   50
  2  \w     30.00  62.00   0.50  115.00    --   94.60 -55.00  -1.00   64
  3  \w      2.00  31.00   0.50   25.00    --    0.00 -82.00-180.00   58
  4  \w    -31.00  28.00   0.50   25.00    --    0.00 -82.00 -60.00  118
  5  \w     -5.00  30.00   0.50   25.00    --    0.00 -82.00  60.00   70
  6  \w      6.00  92.00   0.50  115.00    --   94.60 -30.00 150.00  172
  7  \w     82.00 157.00   0.50  115.00    --   94.60  77.00  90.00  150
  8  \w    136.00 175.00   0.50  115.00    --   94.60  82.00  30.00   78
  9  \w     79.00 177.00   0.50  115.00    --   94.60  45.00-180.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0771390000
_diffrn_orient_matrix_UB_12      -0.0181862000
_diffrn_orient_matrix_UB_13      0.0143115000
_diffrn_orient_matrix_UB_21      -0.0261605000
_diffrn_orient_matrix_UB_22      -0.0579819000
_diffrn_orient_matrix_UB_23      0.0389392000
_diffrn_orient_matrix_UB_31      0.0017875000
_diffrn_orient_matrix_UB_32      -0.0541094000
_diffrn_orient_matrix_UB_33      -0.0462823000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15667
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.113
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2761
_reflns_number_total             4489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07932c2.cif
_cod_data_source_block           20180605_8
_cod_depositor_comments
'Adding full bibliography for 7122551--7122554.cif.'
_cod_original_cell_volume        8873.8(6)
_cod_database_code               7122553
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00Q(H00Q)
2.b Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B)
2.c Aromatic/amide H refined with riding coordinates:
 N009(H009), C00F(H00F), C00I(H00I), C00K(H00K), C00M(H00M), C00O(H00O),
 C00P(H00P)
2.d Idealised Me refined as rotating group:
 C00S(H00C,H00D,H00E), C00U(H00G,H00H,H00J)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.711
_oxdiff_exptl_absorpt_empirical_full_min 0.485