 
data_mt_842_1m 
###################################################################
#                                                                 #
#   for any questions concerning this structure please contact:   #
#                                                                 #
#   Christoph W\"olper                                            #
#   Fachbereich Chemie der                                        #
#   Universit\"at Duisburg-Essen                                  #
#   Campus Essen Universit\"atsstr. 7                             #
#   D-45117 Essen, Germany                                        #
#                                                                 #
#   e-mail: christoph.woelper@uni-due.de                          #
#   phone:  ++49 (0)201 183 4780                                  #
#                                                                 #
###################################################################

loop_
 _publ_author_name
 _publ_author_address
   'Thiele, Maike'
;
   Fachbereich Chemie der
   Universität Duisburg-Essen
   Campus Essen Universitätsstr. 7
   D-45117 Essen, Germany
; 
   'Wölper, Christoph'
;
   Fachbereich Chemie der
   Universität Duisburg-Essen
   Campus Essen Universitätsstr. 7
   D-45117 Essen, Germany
; 
   'Niemeyer, Jochen'
;
   Fachbereich Chemie der
   Universität Duisburg-Essen
   Campus Essen Universitätsstr. 7
   D-45117 Essen, Germany
; 


_publ_section_title
;
 ?
;
_publ_requested_journal           '?'
_journal_name_full                   
;
 ?
;
_journal_coden_Cambridge             353
_journal_year                        ?
_journal_volume                      ?
_journal_issue                       ?
_journal_page_first                  ?
_journal_page_last                   ?
_journal_paper_doi                   ?

_database_code_depnum_ccdc_archive   ?
  
_audit_creation_method            'SHELXL-2017/1' 
_shelx_SHELXL_version_number      '2017/1' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C52 H60 O11' 
_chemical_formula_weight          861.00 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_space_group_crystal_system       tetragonal 
_space_group_IT_number            92 
_space_group_name_H-M_alt         'P 41 21 2' 
_space_group_name_Hall            'P 4abw 2nw' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 '-y+1/2, x+1/2, z+1/4' 
 'y+1/2, -x+1/2, z+3/4' 
 '-x+1/2, y+1/2, -z+1/4' 
 'x+1/2, -y+1/2, -z+3/4' 
 'y, x, -z' 
 '-y, -x, -z+1/2' 
  
_cell_length_a                    9.7530(5) 
_cell_length_b                    9.7530(5) 
_cell_length_c                    46.740(2) 
_cell_angle_alpha                 90 
_cell_angle_beta                  90 
_cell_angle_gamma                 90 
_cell_volume                      4445.9(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     9822 
_cell_measurement_theta_min       3.78 
_cell_measurement_theta_max       79.56 
  
_exptl_crystal_description        prism 
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.286 
_exptl_crystal_F_000              1840 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.644 
_exptl_crystal_size_mid           0.204 
_exptl_crystal_size_min           0.196 
_exptl_absorpt_coefficient_mu     0.725 
_shelx_estimated_absorpt_T_min    0.652 
_shelx_estimated_absorpt_T_max    0.871 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.63 
_exptl_absorpt_correction_T_max   0.75 
_exptl_absorpt_process_details    'SADABS, Blessing, Acta Cryst 1995 A51 33-38' 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_source                    'micro-focus sealed tube' 
_diffrn_measurement_device_type   'Bruker D8 Venture (Photon II detector)' 
_diffrn_source_type               'INCOATEC I\mS 3.0'
_diffrn_radiation_monochromator   'multilayer mirror' 
_diffrn_measurement_method        'Data collection strategy APEX 3/Queen' 
_diffrn_detector_area_resol_mean  7.3910 
_diffrn_reflns_number             217218 
_diffrn_reflns_av_unetI/netI      0.0133 
_diffrn_reflns_av_R_equivalents   0.0632 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -53 
_diffrn_reflns_limit_l_max        59 
_diffrn_reflns_theta_min          3.783 
_diffrn_reflns_theta_max          79.596 
_diffrn_reflns_theta_full         67.679 
_diffrn_measured_fraction_theta_max   0.999 
_diffrn_measured_fraction_theta_full  1.000 
_diffrn_reflns_Laue_measured_fraction_max    0.999 
_diffrn_reflns_Laue_measured_fraction_full   1.000 
_diffrn_reflns_point_group_measured_fraction_max   0.999 
_diffrn_reflns_point_group_measured_fraction_full  1.000 
_reflns_number_total              4853 
_reflns_number_gt                 4801 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.656 
_reflns_Friedel_fraction_max      0.998 
_reflns_Friedel_fraction_full     1.000 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'Bruker APEX3(v2017.3-0)' 
_computing_cell_refinement        'Bruker APEX3(v2017.3-0)' 
_computing_data_reduction         'Bruker APEX3(v2017.3-0)' 
_computing_structure_solution     'Bruker APEX3(v2017.3-0)' 
_computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' 
_computing_molecular_graphics     'ORTEP/PLATON (Spek)' 
_computing_publication_material   'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' 
_refine_special_details           
;
 Treatment of hydrogen atoms:    
 Riding model on idealized geometries 
 with the 1.2 fold isotropic displacement 
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 The methyl groups are idealized with
 tetrahedral angles in a combined 
 rotating and rigid group refinement
 with the 1.5 fold isotropic displacement
 parameters of the equivalent Uij of the 
 corresponding carbon atom.
 Disorder:
 The polyether chain is parially disordered. The corresponding bond lengths and
 angles were restrained to be equal. RIGU and SIMU restraints were applied to
 the displacement parameters of the disordered atoms.
; 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0436P)²+1.3502P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        . 
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1884 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
; 
_refine_ls_abs_structure_Flack    0.11(2) 
_chemical_absolute_configuration  ? 
_refine_ls_number_reflns          4853 
_refine_ls_number_parameters      298 
_refine_ls_number_restraints      8 
_refine_ls_R_factor_all           0.0334 
_refine_ls_R_factor_gt            0.0331 
_refine_ls_wR_factor_ref          0.0908 
_refine_ls_wR_factor_gt           0.0905 
_refine_ls_goodness_of_fit_ref    1.110 
_refine_ls_restrained_S_all       1.109 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
O1 O 0.95137(13) 0.88072(13) 0.03314(2) 0.0211(3) Uani 1 1 d . . . . . 
O2 O 1.01060(15) 0.66782(14) 0.05292(3) 0.0274(3) Uani 1 1 d . . . . . 
O3 O 1.00117(14) 1.28703(14) 0.13807(3) 0.0269(3) Uani 1 1 d . . . . . 
O4 O 1.30139(15) 1.24638(15) 0.12988(3) 0.0293(3) Uani 1 1 d . . . . . 
O5 O 1.40720(16) 1.25675(16) 0.07138(3) 0.0329(3) Uani 1 1 d D . . . . 
O6 O 1.3876(2) 1.3876(2) 0.000000 0.0624(9) Uani 1 2 d S T P A . 
C1 C 0.74097(18) 0.81923(18) 0.01101(3) 0.0196(3) Uani 1 1 d . . . . . 
C2 C 0.80946(18) 0.88419(18) 0.03301(3) 0.0191(3) Uani 1 1 d . . . . . 
C3 C 0.73756(19) 0.96124(18) 0.05428(3) 0.0207(3) Uani 1 1 d . . . . . 
C4 C 0.59801(19) 0.96939(19) 0.05260(4) 0.0222(4) Uani 1 1 d . . . . . 
H4 H 0.549467 1.017471 0.067087 0.027 Uiso 1 1 calc R U . . . 
C5 C 0.52363(19) 0.90856(19) 0.03000(4) 0.0217(4) Uani 1 1 d . . . . . 
C6 C 0.3804(2) 0.9302(2) 0.02698(4) 0.0248(4) Uani 1 1 d . . . . . 
H6 H 0.332332 0.981277 0.041086 0.030 Uiso 1 1 calc R U . . . 
C7 C 0.3108(2) 0.8783(2) 0.00401(4) 0.0276(4) Uani 1 1 d . . . . . 
H7 H 0.215435 0.895480 0.001912 0.033 Uiso 1 1 calc R U . . . 
C8 C 0.3813(2) 0.7991(2) -0.01660(4) 0.0290(4) Uani 1 1 d . . . . . 
H8 H 0.332471 0.762167 -0.032416 0.035 Uiso 1 1 calc R U . . . 
C9 C 0.5190(2) 0.7748(2) -0.01406(4) 0.0241(4) Uani 1 1 d . . . . . 
H9 H 0.564102 0.719379 -0.027880 0.029 Uiso 1 1 calc R U . . . 
C10 C 0.59544(18) 0.83127(19) 0.00898(3) 0.0205(3) Uani 1 1 d . . . . . 
C11 C 1.01270(19) 0.80937(19) 0.05658(4) 0.0237(4) Uani 1 1 d . . . . . 
H11A H 1.108883 0.840134 0.058744 0.028 Uiso 1 1 calc R U . . . 
H11B H 0.963136 0.832999 0.074399 0.028 Uiso 1 1 calc R U . . . 
C12 C 1.1035(2) 0.6210(2) 0.03143(4) 0.0292(4) Uani 1 1 d . . . . . 
H12A H 1.084564 0.668751 0.013407 0.044 Uiso 1 1 calc R U . . . 
H12B H 1.091743 0.522059 0.028676 0.044 Uiso 1 1 calc R U . . . 
H12C H 1.197828 0.639979 0.037443 0.044 Uiso 1 1 calc R U . . . 
C13 C 0.81100(18) 1.04005(18) 0.07700(4) 0.0212(3) Uani 1 1 d . . . . . 
C14 C 0.77295(19) 1.02854(19) 0.10573(4) 0.0220(3) Uani 1 1 d . . . . . 
H14 H 0.703675 0.964924 0.111018 0.026 Uiso 1 1 calc R U . . . 
C15 C 0.83510(19) 1.10909(19) 0.12687(4) 0.0223(3) Uani 1 1 d . . . . . 
C16 C 0.93718(19) 1.20121(19) 0.11842(4) 0.0221(4) Uani 1 1 d . . . . . 
C17 C 0.97287(19) 1.21923(19) 0.08966(4) 0.0228(4) Uani 1 1 d . . . . . 
C18 C 0.91089(19) 1.13518(19) 0.06942(4) 0.0223(4) Uani 1 1 d . . . . . 
H18 H 0.937393 1.142891 0.049932 0.027 Uiso 1 1 calc R U . . . 
C19 C 0.7880(2) 1.0990(2) 0.15752(4) 0.0274(4) Uani 1 1 d . . . . . 
H19A H 0.693479 1.064877 0.158055 0.041 Uiso 1 1 calc R U . . . 
H19B H 0.791969 1.189806 0.166445 0.041 Uiso 1 1 calc R U . . . 
H19C H 0.847797 1.035683 0.167971 0.041 Uiso 1 1 calc R U . . . 
C20 C 1.0710(2) 1.3296(2) 0.08061(4) 0.0288(4) Uani 1 1 d . . . . . 
H20A H 1.090513 1.320349 0.060133 0.043 Uiso 1 1 calc R U . . . 
H20B H 1.156459 1.320740 0.091485 0.043 Uiso 1 1 calc R U . . . 
H20C H 1.030104 1.419611 0.084308 0.043 Uiso 1 1 calc R U . . . 
C21 C 1.0962(2) 1.2218(2) 0.15738(4) 0.0311(4) Uani 1 1 d . . . . . 
H21A H 1.045139 1.154517 0.169120 0.037 Uiso 1 1 calc R U . . . 
H21B H 1.133200 1.292352 0.170513 0.037 Uiso 1 1 calc R U . . . 
C22 C 1.2146(2) 1.1494(2) 0.14334(4) 0.0289(4) Uani 1 1 d . . . . . 
H22A H 1.267089 1.097594 0.157889 0.035 Uiso 1 1 calc R U . . . 
H22B H 1.179753 1.083543 0.128964 0.035 Uiso 1 1 calc R U . . . 
C23 C 1.4247(2) 1.1860(2) 0.11950(4) 0.0312(4) Uani 1 1 d . . . . . 
H23A H 1.405071 1.094365 0.111347 0.037 Uiso 1 1 calc R U . . . 
H23B H 1.490881 1.174670 0.135391 0.037 Uiso 1 1 calc R U . . . 
C24 C 1.4846(2) 1.2778(2) 0.09684(4) 0.0323(4) Uani 1 1 d . . . . . 
H24A H 1.478849 1.374917 0.102885 0.039 Uiso 1 1 calc R U . . . 
H24B H 1.582150 1.254582 0.093541 0.039 Uiso 1 1 calc R U . . . 
C25 C 1.4605(11) 1.3197(16) 0.0467(2) 0.034(2) Uani 0.45(3) 1 d D U P A 1 
H25A H 1.548171 1.275544 0.041276 0.041 Uiso 0.45(3) 1 calc R U P A 1 
H25B H 1.478627 1.417847 0.050528 0.041 Uiso 0.45(3) 1 calc R U P A 1 
C25' C 1.4272(11) 1.3573(10) 0.05033(16) 0.0320(16) Uani 0.55(3) 1 d D U P A 2 
H25C H 1.526382 1.373360 0.047349 0.038 Uiso 0.55(3) 1 calc R U P A 2 
H25D H 1.384249 1.444709 0.056317 0.038 Uiso 0.55(3) 1 calc R U P A 2 
C26 C 1.3627(3) 1.3067(2) 0.02336(4) 0.0376(5) Uani 1 1 d D . . . . 
H26A H 1.361226 1.209800 0.017057 0.045 Uiso 0.45(3) 1 calc R U P A 1 
H26B H 1.270252 1.328886 0.030789 0.045 Uiso 0.45(3) 1 calc R U P A 1 
H26C H 1.397054 1.213125 0.019369 0.045 Uiso 0.55(3) 1 calc R U P A 2 
H26D H 1.262337 1.300354 0.026268 0.045 Uiso 0.55(3) 1 calc R U P A 2 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
O1 C2 1.385(2) . ? 
O1 C11 1.429(2) . ? 
O2 C11 1.391(2) . ? 
O2 C12 1.428(2) . ? 
O3 C16 1.391(2) . ? 
O3 C21 1.441(2) . ? 
O4 C22 1.416(2) . ? 
O4 C23 1.424(2) . ? 
O5 C25' 1.403(7) . ? 
O5 C25 1.408(9) . ? 
O5 C24 1.424(2) . ? 
O6 C26 1.368(3) 7 ? 
O6 C26 1.368(3) . ? 
C1 C2 1.380(2) . ? 
C1 C10 1.427(2) . ? 
C1 C1 1.491(3) 7 ? 
C2 C3 1.430(2) . ? 
C3 C4 1.366(3) . ? 
C3 C13 1.494(2) . ? 
C4 C5 1.412(2) . ? 
C5 C6 1.420(3) . ? 
C5 C10 1.423(2) . ? 
C6 C7 1.367(3) . ? 
C7 C8 1.414(3) . ? 
C8 C9 1.369(3) . ? 
C9 C10 1.421(2) . ? 
C13 C18 1.391(3) . ? 
C13 C14 1.398(2) . ? 
C14 C15 1.400(2) . ? 
C15 C16 1.398(3) . ? 
C15 C19 1.508(2) . ? 
C16 C17 1.400(2) . ? 
C17 C18 1.390(2) . ? 
C17 C20 1.501(3) . ? 
C21 C22 1.504(3) . ? 
C23 C24 1.505(3) . ? 
C25 C26 1.454(9) . ? 
C25' C26 1.493(7) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 O1 C11 115.69(13) . . ? 
C11 O2 C12 113.25(15) . . ? 
C16 O3 C21 115.89(15) . . ? 
C22 O4 C23 112.32(16) . . ? 
C25' O5 C24 114.3(3) . . ? 
C25 O5 C24 115.3(4) . . ? 
C26 O6 C26 115.6(3) 7 . ? 
C2 C1 C10 119.54(15) . . ? 
C2 C1 C1 120.09(15) . 7 ? 
C10 C1 C1 120.34(14) . 7 ? 
C1 C2 O1 118.41(15) . . ? 
C1 C2 C3 121.46(16) . . ? 
O1 C2 C3 120.01(15) . . ? 
C4 C3 C2 118.65(16) . . ? 
C4 C3 C13 119.26(16) . . ? 
C2 C3 C13 121.97(16) . . ? 
C3 C4 C5 122.04(16) . . ? 
C4 C5 C6 121.16(17) . . ? 
C4 C5 C10 119.10(16) . . ? 
C6 C5 C10 119.63(17) . . ? 
C7 C6 C5 120.77(18) . . ? 
C6 C7 C8 119.74(18) . . ? 
C9 C8 C7 120.83(18) . . ? 
C8 C9 C10 120.89(17) . . ? 
C9 C10 C5 118.08(16) . . ? 
C9 C10 C1 122.70(16) . . ? 
C5 C10 C1 119.15(16) . . ? 
O2 C11 O1 112.49(14) . . ? 
C18 C13 C14 118.95(16) . . ? 
C18 C13 C3 119.87(15) . . ? 
C14 C13 C3 120.95(17) . . ? 
C13 C14 C15 121.19(17) . . ? 
C16 C15 C14 118.01(16) . . ? 
C16 C15 C19 121.84(16) . . ? 
C14 C15 C19 120.11(17) . . ? 
O3 C16 C15 121.33(16) . . ? 
O3 C16 C17 116.56(17) . . ? 
C15 C16 C17 121.94(16) . . ? 
C18 C17 C16 118.12(17) . . ? 
C18 C17 C20 120.56(16) . . ? 
C16 C17 C20 121.28(17) . . ? 
C17 C18 C13 121.65(16) . . ? 
O3 C21 C22 115.31(15) . . ? 
O4 C22 C21 109.83(17) . . ? 
O4 C23 C24 108.74(17) . . ? 
O5 C24 C23 107.25(18) . . ? 
O5 C25 C26 109.5(6) . . ? 
O5 C25' C26 107.6(5) . . ? 
O6 C26 C25 115.5(4) . . ? 
O6 C26 C25' 114.1(3) . . ? 
  
_refine_diff_density_max    0.214 
_refine_diff_density_min   -0.229 
_refine_diff_density_rms    0.035 
  
  
  
