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_7039294
_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         'C31 H45 K O5'
_chemical_formula_sum            'C31 H45 K O5'
_chemical_formula_weight         536.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-12
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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2016-03-02 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.614(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.1093(3)
_cell_length_b                   26.4085(9)
_cell_length_c                   20.4600(7)
_cell_measurement_reflns_used    3684
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      28.3900
_cell_measurement_theta_min      3.9750
_cell_volume                     5996.3(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details
;
  1 omega   -9.00   25.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571  -99.0000 -120.0000 34

  2 omega  -19.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -57.0000  150.0000 59

  3 omega  -45.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946    0.0000    0.0000 113
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
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_diffrn_orient_matrix_UB_12      0.0231760000
_diffrn_orient_matrix_UB_13      -0.0159493000
_diffrn_orient_matrix_UB_21      -0.0114863000
_diffrn_orient_matrix_UB_22      0.0112016000
_diffrn_orient_matrix_UB_23      0.0306068000
_diffrn_orient_matrix_UB_31      0.0611650000
_diffrn_orient_matrix_UB_32      0.0076481000
_diffrn_orient_matrix_UB_33      0.0035997000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_k_min       -32
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_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12487
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.838
_diffrn_reflns_theta_min         3.365
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
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_exptl_crystal_F_000             2320
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
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_refine_diff_density_max         0.499
_refine_diff_density_min         -0.328
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6823
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0497
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+5.9552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5106
_reflns_number_total             6823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01417h2.cif
_cod_data_source_block           lyg_k_0115
_cod_depositor_comments
'Adding full bibliography for 7039292--7039295.cif.'
_cod_database_code               7039294
_reflns_odcompleteness_completeness 99.74
_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. Rigid bond restraints
 C15, C16, C17, C18, C16', C17', C18'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C16' \\sim C17' \\sim C18': within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Sof(C16')=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17')=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C11(H11)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C16'(H16D,H16E,
 H16F), C17'(H17D,H17E,H17F), C18'(H18D,H18E,H18F), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              13641
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method tetrahydrofuran