An Asymmetric Cryptand for the Site-Specific Coordination of 3d Metals in Multiple Oxidation States
Jökel, Julia; Nyßen, Frauke; Siegmund, Daniel; Apfel, Ulf-Peter; Dalton Transactions  (2021) –; doi:10.1039/D1DT02075G

data_7708409
_publ_section_title
;
 An Asymmetric Cryptand for the Site-Specific Coordination of 3d Metals in
 Multiple Oxidation States
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02075G
_journal_year                    2021
_chemical_formula_moiety         '4(Cl O4), C36 H55 N5 S3, 2(H2 O)'
_chemical_formula_sum            'C36 H59 Cl4 N5 O18 S3'
_chemical_formula_weight         1087.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.771(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3506(5)
_cell_length_b                   28.6229(14)
_cell_length_c                   17.3038(8)
_cell_measurement_reflns_used    12707
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.5720
_cell_measurement_theta_min      3.2350
_cell_volume                     5124.0(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -129.50   68.50   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000    1.0000  290.0000 198

  2 omega  -79.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   11.0000  280.0000 196

  3 phi    300.00  330.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -40.0000 -109.0000     -     30

  4 omega  -24.50   34.50   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   91.0000   90.0000 59

  5 omega   32.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000 -179.0000  340.0000 106

  6 omega  -16.50  111.50   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   51.0000    0.0000 128

  7 phi    130.00  160.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -40.0000    1.0000     -     30

  8 omega   11.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000 -129.0000  190.0000 30

  9 omega  -78.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -79.0000  320.0000 139

 10 omega   56.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000  151.0000   20.0000 53
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0253070000
_diffrn_orient_matrix_UB_12      -0.0072148000
_diffrn_orient_matrix_UB_13      -0.0366194000
_diffrn_orient_matrix_UB_21      -0.0007692000
_diffrn_orient_matrix_UB_22      -0.0235128000
_diffrn_orient_matrix_UB_23      0.0130264000
_diffrn_orient_matrix_UB_31      -0.0637046000
_diffrn_orient_matrix_UB_32      0.0031756000
_diffrn_orient_matrix_UB_33      0.0130510000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36004
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.081
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 3536 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      3.634
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+2.9178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                8096
_reflns_number_total             8987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02075g2.cif
_cod_data_source_block           fm-586
_cod_database_code               7708409
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.935
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 Cl4-O13 \\sim Cl4-O14 \\sim Cl4-O15 \\sim Cl4-O16
 with sigma of 0.02
 O13-O15 \\sim O14-O16 \\sim O13-O16 \\sim O14-O15 \\sim O13-O14 \\sim O15-O16
 with sigma of 0.04
 Cl4-O13 \\sim Cl4-O14A
 with sigma of 0.02
 Cl4-O15 \\sim Cl4-O13A
 with sigma of 0.02
 Cl4-O14 \\sim Cl4-O17
 with sigma of 0.02
 Cl4-O16 \\sim Cl4-O15A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O9 \\sim O10 \\sim O11 \\sim O12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Cl4 \\sim O13 \\sim O14 \\sim O15 \\sim O16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O14 \\sim O14A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
Uanis(O15A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 Cl4, O13, O14, O15, O16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O14A)=Sof(O13A)=Sof(O15A)=Sof(O16A)=Sof(O17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=Sof(O17)=Sof(H17A)=Sof(H17B)=FVAR(1)
5.a Free rotating group:
 O19(H19A,H19B), Cl4(O13,O14,O15,O16,O17,H17A,H17B), O17A(H17C,H17D)
5.b Ternary CH refined with riding coordinates:
 N1(H1)
5.c Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), C1(H1A,H1B), C2(H2A,H2B), C3(H3C,H3D),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
  C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C9(H9), C17(H17), C18(H18), C19(H19), C21(H21),
 C29(H29), C30(H30), C31(H31), C33(H33)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95058
_shelx_fab_checksum              35788
_olex2_submission_special_instructions 'No special instructions were received'