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_7039292
_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_absolute_configuration ad
_chemical_formula_moiety         'C52 H68 K2 O7, C52 H70 K2 O8, 4(C2 H3 N)'
_chemical_formula_sum            'C112 H150 K4 N4 O15'
_chemical_formula_weight         1948.76
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-14
_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                 109.1440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4859(10)
_cell_length_b                   20.6897(15)
_cell_length_c                   20.2255(15)
_cell_measurement_reflns_used    8908
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      2.35
_cell_volume                     5331.2(7)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.696
_diffrn_measured_fraction_theta_max 0.670
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.1242
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27252
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.36
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2092
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         15886
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                10309
_reflns_number_total             15886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01417h2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7039292--7039295.cif.'
_cod_database_code               7039292
_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, All O(H,H) groups
2. Rigid bond restraints
 C81, C82, C82A, C83, C83A, C84, C84A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, C34, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30, C31, C32
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
C81 \\sim C82 \\sim C82A \\sim C83 \\sim C83A \\sim C84 \\sim C84A: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C29 \\sim C30 \\sim C31 \\sim C32: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
4. Others
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=1-FVAR(1)
 Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C83A)=Sof(H83D)=Sof(H83E)=
 Sof(H83F)=Sof(C84A)=Sof(H84D)=Sof(H84E)=Sof(H84F)=FVAR(1)
5.a Rotating group:
 O15(H15A,H15B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B), C59(H59A,H59B), C66(H66A,H66B), C73(H73A,
 H73B), C80(H80A,H80B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B),
 C100(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,
 H10J)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11), C13(H13), C18(H18), C20(H20), C25(H25), C27(H27),
 C55(H55), C57(H57), C63(H63), C65(H65), C70(H70), C72(H72), C77(H77), C79(H79)
5.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C82(H82A,H82B,H82C), C82A(H82D,H82E,H82F), C83(H83A,H83B,
 H83C), C83A(H83D,H83E,H83F), C84(H84A,H84B,H84C), C84A(H84D,H84E,H84F),
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,
 H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C), C95(H95A,
 H95B,H95C), C96(H96A,H96B,H96C), C105(H10K,H10L,H10M), C107(H10N,H10O,H10P),
 C109(H10Q,H10R,H10S), C111(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method acetonitrile