A pillar[6]arene-based [2]pseudorotaxane in solution and in the solid state and its photo-responsive self-assembly behavior in solution
Danyu Xia; Peifa Wei; Bingbing Shi; Feihe Huang; Chem.Commun. 52 (2016) 513–; doi:

data_7118410
_publ_section_title
;
 A pillar[6]arene-based [2]pseudorotaxane in solution and in the solid
 state and its photo-responsive self-assembly behavior in solution
;
_journal_name_full               Chem.Commun.
_journal_page_first              513
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
C78 H108 O24, C14 H16 N2, 2(F6 P), 1.75(CH3CN)
;
_chemical_formula_sum            'C95.5 H129.25 F12 N3.75 O24 P2'
_chemical_formula_weight         2003.72
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-06-29 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.155(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.6051(11)
_cell_length_b                   13.3823(5)
_cell_length_c                   24.6753(7)
_cell_measurement_reflns_used    10550
_cell_measurement_temperature    171.9
_cell_measurement_theta_max      29.5598
_cell_measurement_theta_min      2.9603
_cell_volume                     10436.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      171.9
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0132226000
_diffrn_orient_matrix_UB_12      0.0047314000
_diffrn_orient_matrix_UB_13      -0.0230401000
_diffrn_orient_matrix_UB_21      -0.0104853000
_diffrn_orient_matrix_UB_22      0.0449750000
_diffrn_orient_matrix_UB_23      -0.0071770000
_diffrn_orient_matrix_UB_31      0.0147972000
_diffrn_orient_matrix_UB_32      0.0276340000
_diffrn_orient_matrix_UB_33      0.0156252000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32316
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4234
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_platon_squeeze_details
;
;
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.13(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         15071
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                12597
_reflns_number_total             15071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc08038j2.cif
_cod_data_source_block           141016_xdy_hg7_3
_cod_original_formula_sum        'C95.50 H129.25 F12 N3.75 O24 P2'
_cod_database_code               7118410
_chemical_oxdiff_formula         'c10 h10 o10 p1 f6'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B),
  C27(H27A,H27B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,
 H38B), C40(H40A,H40B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B),
 C51(H51A,H51B), C53(H53A,H53B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B),
  C64(H64A,H64B), C66(H66A,H66B), C73(H73A,H73B), C74(H74A,H74B), C76(H76A,
 H76B), C77(H77A,H77B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C16(H16), C19(H19), C29(H29), C32(H32), C42(H42), C45(H45),
 C55(H55), C58(H58), C68(H68), C71(H71), C05U(H05U), C79(H79), C80(H80),
 C82(H82), C83(H83), C85(H85), C86(H86), C88(H88), C90(H90), C91(H91)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C52(H52A,
 H52B,H52C), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C75(H75A,H75B,H75C),
 C78(H78A,H78B,H78C), C84(H84A,H84B,H84C), C92(H92A,H92B,H92C)
;