Structures of potassium calix[4]arene crown ether inclusion complexes and application in polymerization of rac-lactide.
Li, Yingguo; Zhao, Hongwei; Mao, Xiaoyang; Pan, Xiaobo; Wu, Jincai; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9636–9645; doi:10.1039/c6dt01417h

data_7039295
_publ_section_title
;
 Structures of potassium calix[4]arene crown ether inclusion complexes and
 application in polymerization of rac-lactide.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9636
_journal_page_last               9645
_journal_paper_doi               10.1039/c6dt01417h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '0.5(C100 H132 K4 O8)'
_chemical_formula_sum            'C50 H66 K2 O4'
_chemical_formula_weight         809.23
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-02 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2579(5)
_cell_length_b                   17.9504(9)
_cell_length_c                   21.1486(6)
_cell_measurement_reflns_used    3091
_cell_measurement_temperature    220.60(10)
_cell_measurement_theta_max      23.2810
_cell_measurement_theta_min      3.9950
_cell_volume                     4653.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.60(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
;
  1 omega  -27.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541  -77.0000  150.0000 74

  2 omega  -18.00   94.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541   19.0000  -30.0000 112

  3 omega   24.00   58.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541   77.0000   60.0000 34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0427965000
_diffrn_orient_matrix_UB_12      0.0254387000
_diffrn_orient_matrix_UB_13      -0.0065435000
_diffrn_orient_matrix_UB_21      0.0327137000
_diffrn_orient_matrix_UB_22      0.0172619000
_diffrn_orient_matrix_UB_23      -0.0234554000
_diffrn_orient_matrix_UB_31      -0.0211521000
_diffrn_orient_matrix_UB_32      -0.0248124000
_diffrn_orient_matrix_UB_33      -0.0230664000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19712
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5681
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+4.6608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2526
_reflns_number_gt                3156
_reflns_number_total             5681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01417h2.cif
_cod_data_source_block           wujc0310_1
_cod_depositor_comments
'Adding full bibliography for 7039292--7039295.cif.'
_cod_database_code               7039295
_reflns_odcompleteness_completeness 99.64
_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. Restrained distances
 C8-C25
 1.54 with sigma of 0.02
 C20-C21
 1.38 with sigma of 0.002
 C8-C26
 1.54 with sigma of 0.02
 C8-C27
 1.54 with sigma of 0.02
 C8-C25'
 1.54 with sigma of 0.02
 C8-C26'
 1.54 with sigma of 0.02
 C8-C27'
 1.54 with sigma of 0.02
 C14-C28 = C14-C29 = C14-C30
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C25, C26, C27, C25', C27', C26'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C23, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
C24 \\sim C23 \\sim C19: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
5. Others
 Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C27')=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C26')=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) H24A(0.5) H24B(0.5)
 H24C(0.5)
6.a Riding coordinates:
 C30(H30A,H30B,H30C)
6.b Ternary CH refined with riding coordinates:
 C3(H3), C17(H17)
6.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C20(H20A,H20B), C21(H21A,H21B)
6.d Me refined with riding coordinates:
 C28(H28A,H28B,H28C)
6.e Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11)
6.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C25'(H25D,H25E,H25F), C27'(H27D,H27E,H27F), C26'(H26D,H26E,H26F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method tetrahydrofuran