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_7122551
_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, 2(C2 H6 O S), 2(N O3)'
_chemical_formula_sum            'C132 H136 F4 N26 O24 Pd2 S2'
_chemical_formula_weight         2823.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c 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            4
_cell_length_a                   21.3685(3)
_cell_length_b                   26.9448(4)
_cell_length_c                   41.0041(8)
_cell_measurement_reflns_used    31972
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.6080
_cell_measurement_theta_min      2.6500
_cell_volume                     23608.9(7)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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     31.00  56.00   0.50    8.00    --    0.00  71.00-117.00   50
  2  \w     10.00  35.00   0.50    8.00    --    0.00  51.00  52.00   50
  3  \w    -59.00 -34.00   0.50    8.00    --    0.00 -51.00 -94.00   50
  4  \w    105.00 130.00   0.50   45.00    --   94.60  51.00  52.00   50
  5  \w     62.00  89.00   0.50   45.00    --   94.60 -71.00 111.00   54
  6  \w     58.00  84.00   0.50   45.00    --   94.60 -51.00 -94.00   52
  7  \w    101.00 126.00   0.50   45.00    --   94.60  71.00-117.00   50
  8  \w    -24.00  27.00   0.50    8.00    --    0.00 -82.00-150.00  102
  9  \w    -31.00  11.00   0.50    8.00    --    0.00 -82.00  60.00   84
 10  \w    -30.00   0.00   0.50    8.00    --    0.00 -82.00 -30.00   60
 11  \w     13.00  93.00   0.50   45.00    --   94.60 -45.00  90.00  160
 12  \w    134.00 183.00   0.50   45.00    --   94.60  30.00  60.00   98
 13  \w     79.00 126.00   0.50   45.00    --   94.60  30.00  60.00   94
 14  \w    137.00 184.00   0.50   45.00    --   94.60  45.00 120.00   94
 15  \w     87.00 137.00   0.50   45.00    --   94.60  82.00-150.00  100
 16  \w     87.00 179.00   0.50   45.00    --   94.60  82.00 -30.00  184
;
_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      0.0118700000
_diffrn_orient_matrix_UB_12      0.0457337000
_diffrn_orient_matrix_UB_13      0.0217771000
_diffrn_orient_matrix_UB_21      0.0702594000
_diffrn_orient_matrix_UB_22      -0.0022607000
_diffrn_orient_matrix_UB_23      -0.0083268000
_diffrn_orient_matrix_UB_31      -0.0111217000
_diffrn_orient_matrix_UB_32      0.0342304000
_diffrn_orient_matrix_UB_33      -0.0294509000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            109782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.891
_diffrn_reflns_theta_min         2.639
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20845
_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    0.794
_exptl_crystal_description       block
_exptl_crystal_F_000             5848
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         23740
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1730P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12485
_reflns_number_total             23740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07932c2.cif
_cod_data_source_block           20180614_2
_cod_depositor_comments
'Adding full bibliography for 7122551--7122554.cif.'
_cod_database_code               7122551
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 99.88
_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. Restrained distances
 O0AA-O2
 2.2 with sigma of 0.02
 O1AA-O2
 2.2 with sigma of 0.02
 N1-O2
 1.12 with sigma of 0.02
 O2-O1AA
 2 with sigma of 0.002
 N1-O1AA
 1.1 with sigma of 0.02
3. Rigid bond restraints
 N00D, C01U
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N00J, C01F
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N00P, C01H
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C12, C02D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C01O, C028
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C01E, C01I
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C02L) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C024(H024), C025(H025), C02D(H02K), C02K(H02W)
5.b Secondary CH2 refined with riding coordinates:
 C01V(H01C,H01D), C021(H02A,H02B), C023(H02C,H02D), C02A(H02E,H02F)
5.c Aromatic/amide H refined with riding coordinates:
 N00C(H00C), N00E(H00E), N00K(H00K), C00S(H00S), N00W(H00W), C00Z(H00Z),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01H(H01H), C01I(H01I),
 C01K(H01K), C01O(H01O), C01T(H01T), C01U(H01U), C01X(H01X), C026(H026),
 C027(H027), C028(H028), C029(H029), C02C(H02J), C02G(H02O), C02J(H02V),
 C02L(H02X), C02M(H02Y)
5.d Idealised Me refined as rotating group:
 C01S(H01J,H01L,H01M), C01Z(H01E,H01F,H01G), C02B(H02G,H02H,H02I), C02E(H02L,
 H02M,H02N), C02F(H0AA,H,HA), C02H(H02P,H02Q,H02R), C02I(H02S,H02T,H02U),
 C02O(H02Z,HB,HC), C02V(H02,HD,HE), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              49057
_shelx_hkl_checksum              59714
_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 3.174
_oxdiff_exptl_absorpt_empirical_full_min 0.554