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_7039293
_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         'C56 H77 K O8, 5(C4 H8 O)'
_chemical_formula_sum            'C76 H117 K O13'
_chemical_formula_weight         1277.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-02 deposited with the CCDC.
2016-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8725(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3022(3)
_cell_length_b                   29.2158(5)
_cell_length_c                   15.5007(3)
_cell_measurement_reflns_used    7186
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.3810
_cell_measurement_theta_min      4.0450
_cell_volume                     7356.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
  1 omega  -85.00  -50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  178.0000  120.0000 35

  2 omega  -87.00  -62.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  178.0000   60.0000 25

  3 omega  -58.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  111.0000  150.0000 48

  4 omega  -85.00  -34.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  178.0000 -150.0000 51

  5 omega   22.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 102

  6 omega   28.00   64.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  150.0000 36

  7 omega   91.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  150.0000 36

  8 omega   28.00   73.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   90.0000 45

  9 omega  103.00  174.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 71

 10 omega   72.00  103.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 31

 11 omega   95.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -180.0000 25

 12 omega   49.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  150.0000 55

 13 omega   93.00  169.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -150.0000 76

 14 omega   91.00  129.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000 -120.0000 38

 15 omega  108.00  164.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 56

 16 omega   91.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -90.0000 48

 17 omega   34.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 60

 18 omega  102.00  136.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 34

 19 omega  107.00  166.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -120.0000 59

 20 omega   57.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   60.0000 34

 21 omega   52.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 25

 22 omega   42.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -30.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0122129000
_diffrn_orient_matrix_UB_12      0.0382458000
_diffrn_orient_matrix_UB_13      0.0661283000
_diffrn_orient_matrix_UB_21      0.0925433000
_diffrn_orient_matrix_UB_22      0.0112831000
_diffrn_orient_matrix_UB_23      0.0038629000
_diffrn_orient_matrix_UB_31      -0.0167840000
_diffrn_orient_matrix_UB_32      0.0344882000
_diffrn_orient_matrix_UB_33      -0.0745994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30815
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.650
_diffrn_reflns_theta_min         4.070
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93554
_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.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         13341
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+2.8822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9893
_reflns_number_total             13341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01417h2.cif
_cod_data_source_block           liyguo0908_2
_cod_depositor_comments
'Adding full bibliography for 7039292--7039295.cif.'
_cod_database_code               7039293
_reflns_odcompleteness_completeness 97.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65'-C68'
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C72) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(C34')=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35')=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C36')=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C42')=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C43')=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C44')=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(2)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(2)
 Sof(O10')=Sof(C65')=Sof(H65C)=Sof(H65D)=Sof(C66')=Sof(H66C)=Sof(H66D)=
 Sof(C67')=Sof(H67C)=Sof(H67D)=Sof(C68')=Sof(H68C)=Sof(H68D)=1-FVAR(3)
 Sof(O10)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=
 Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(3)
5.a 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), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
 C68(H68A,H68B), C65'(H65C,H65D), C66'(H66C,H66D), C67'(H67C,H67D), C68'(H68C,
 H68D), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C69(H69A,H69B),
  C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,
 H74B), C75(H75A,H75B), C76(H76A,H76B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25)
5.c Fitted pentagon refined as free rotating group:
 O12(C61,C62,C63,C64), O11(C69,C70,C71,C72), O13(C73,C74,C75,C76)
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), C34'(H34D,H34E,H34F),
 C35'(H35D,H35E,H35F), C36'(H36D,H36E,H36F), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C42'(H42D,H42E,H42F), C43'(H43D,H43E,H43F), C44'(H44D,H44E,H44F)
;
_shelx_res_checksum              92892
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method tetrahydrofuran