Formation of a [2]pseudorotaxane based on a pillar[5]arene and a rigid guest in solution and in the solid state
Yujuan Zhou; Zhengtao Li; Xiaodong Chi; Connor Thompson; Yong Yao; Chem.Commun. 50 (2014) 10482–; doi:10.1039/C4cc04319G

data_7115559
_publ_section_title
;
 Formation of a [2]pseudorotaxane based on a pillar[5]arene and a rigid
 guest in solution and in the solid state
;
_journal_name_full               Chem.Commun.
_journal_page_first              10482
_journal_paper_doi               10.1039/C4cc04319G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'4(F6 P), 2(C65 H90 O20), 2(C16 H14 N2), 3(C2 H3 N)'
_chemical_formula_sum            'C168 H217 F24 N7 O40 P4'
_chemical_formula_weight         3554.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                104.590(3)
_cell_angle_beta                 100.420(4)
_cell_angle_gamma                95.616(3)
_cell_formula_units_Z            1
_cell_length_a                   12.6852(6)
_cell_length_b                   17.3581(6)
_cell_length_c                   21.7669(9)
_cell_measurement_reflns_used    7001
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      29.5640
_cell_measurement_theta_min      3.0180
_cell_volume                     4509.7(3)
_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      170.1
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0553690000
_diffrn_orient_matrix_UB_12      -0.0050619000
_diffrn_orient_matrix_UB_13      0.0033717000
_diffrn_orient_matrix_UB_21      -0.0153873000
_diffrn_orient_matrix_UB_22      -0.0404269000
_diffrn_orient_matrix_UB_23      -0.0194186000
_diffrn_orient_matrix_UB_31      0.0022117000
_diffrn_orient_matrix_UB_32      0.0128207000
_diffrn_orient_matrix_UB_33      -0.0282743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30719
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92687
_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    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1122
_refine_ls_number_reflns         18372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+2.0735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2313
_reflns_number_gt                11015
_reflns_number_total             18372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04319g2.cif
_cod_data_source_block           140424_h+g20
_cod_database_code               7115559
_chemical_oxdiff_formula         'c10 h10 n2 o8 p1 f6'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H12A,H12B,H12C} of C12, All C(H,H) groups
 At 1.5 times of:
  {H1UA,H1UB,H1UC} of C1U, {H19A,H19B,H19C} of C19, {H80A,H80B,H80C} of C80,
  {H1JA,H1JB,H1JC} of C1J, {H1OA,H1OB,H1OC} of C1O, {H7A,H7B,H7C} of C7, {H37A,
  H37B,H37C} of C37, {H11A,H11B,H11C} of C11, {H78A,H78B,H78C} of C78, {H74A,
  H74B,H74C} of C74, {H62A,H62B,H62C} of C62, {H52A,H52B,H52C} of C52, {H45A,
  H45B,H45C} of C45
2. Others
 Fixed Sof: C1Q(0.5) C1U(0.5) H1UA(0.5) H1UB(0.5) H1UC(0.5) N1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C4(H4A,H4B), C41(H41A,H41B), C2(H2A,H2B), C27(H27A,H27B),
 C66(H66A,H66B), C25(H25A,H25B), C34(H34A,H34B), C32(H32A,H32B), C14(H14A,H14B),
  C76(H76A,H76B), C64(H64A,H64B), C1(H1A,H1B), C3(H3A,H3B), C33(H33A,H33B),
 C65(H65A,H65B), C72(H72A,H72B), C58(H58A,H58B), C71(H71A,H71B), C40(H40A,H40B),
  C63(H63A,H63B), C42(H42A,H42B), C69(H69A,H69B), C1S(H1SA,H1SB), C48(H48A,H48B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C60(H60), C8(H8), C22(H22), C29(H29), C51(H51), C43(H43), C6(H6),
 C24(H24), C54(H54), C1E(H1E), C1F(H1F), C1H(H1H), C1I(H1I), C1K(H1K), C1L(H1L),
  C1M(H1M), C1N(H1N)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C37(H37A,H37B,H37C), C11(H11A,H11B,H11C), C78(H78A,H78B,
 H78C), C74(H74A,H74B,H74C), C62(H62A,H62B,H62C), C52(H52A,H52B,H52C), C45(H45A,
 H45B,H45C), C1J(H1JA,H1JB,H1JC), C1O(H1OA,H1OB,H1OC), C12(H12A,H12B,H12C),
 C80(H80A,H80B,H80C), C19(H19A,H19B,H19C), C1U(H1UA,H1UB,H1UC)
;