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_7708410
_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         '2(C36 H53 Cu N5 S3), 7(Cl), 4(C H4 O)'
_chemical_formula_sum            'C76 H122 Cl7 Cu2 N10 O4 S6'
_chemical_formula_weight         1807.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                66.345(3)
_cell_angle_beta                 81.345(3)
_cell_angle_gamma                69.195(3)
_cell_formula_units_Z            1
_cell_length_a                   12.4346(4)
_cell_length_b                   13.9327(4)
_cell_length_c                   15.5273(6)
_cell_measurement_reflns_used    21579
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      74.5810
_cell_measurement_theta_min      3.6260
_cell_volume                     2303.27(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -71.00  30.00   1.00    5.00    --  -42.65  57.00 120.00  101
  2  \w   -115.00 -15.00   1.00    5.00    --  -42.65 -57.00 -30.00  100
  3  \w    -20.00  84.00   1.00    5.00    --   42.65 -99.00-120.00  104
  4  \w     32.00 137.00   1.00   17.50    --  108.66 -30.00 -30.00  105
  5  \w     80.00 158.00   1.00   17.50    --  108.66  30.00-150.00   78
  6  \w     35.00 122.00   1.00   17.50    --  108.66-125.00 120.00   87
  7  \w     73.00 158.00   1.00   17.50    --  108.66 125.00 120.00   85
  8  \w     32.00 137.00   1.00   17.50    --  108.66 -30.00-180.00  105
  9  \w     80.00 158.00   1.00   17.50    --  108.66  30.00-180.00   78
 10  \w     33.00 141.00   1.00   17.50    --  108.66 -77.00 -90.00  108
 11  \w     33.00 141.00   1.00   17.50    --  108.66 -77.00 120.00  108
 12  \w   -119.00 -10.00   1.00    5.00    --  -42.65 -77.00 120.00  109
 13  \w   -115.00 -15.00   1.00    5.00    --  -42.65 -57.00-150.00  100
 14  \w    -29.00  71.00   1.00    5.00    --   42.65 -57.00 -30.00  100
 15  \w     80.00 158.00   1.00   17.50    --  108.66  61.00 -90.00   78
 16  \w     83.00 158.00   1.00   17.50    --  108.66  45.00  60.00   75
 17  \w     80.00 158.00   1.00   17.50    --  108.66  30.00 120.00   78
 18  \w     76.00 158.00   1.00   17.50    --  108.66  77.00   0.00   82
 19  \w     76.00 158.00   1.00   17.50    --  108.66  77.00 -60.00   82
 20  \w     80.00 158.00   1.00   17.50    --  108.66  30.00   0.00   78
 21  \w   -119.00 -10.00   1.00    5.00    --  -42.65 -77.00-180.00  109
 22  \w   -119.00 -10.00   1.00    5.00    --  -42.65 -77.00  30.00  109
 23  \w   -119.00 -10.00   1.00    5.00    --  -42.65 -77.00 -90.00  109
 24  \w     76.00 158.00   1.00   17.50    --  108.66  77.00 -30.00   82
 25  \w     80.00 158.00   1.00   17.50    --  108.66  61.00 120.00   78
 26  \w     76.00 126.00   1.00   17.50    --  108.66  77.00-180.00   50
 27  \w     83.00 158.00   1.00   17.50    --  108.66  45.00-120.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0907624000
_diffrn_orient_matrix_UB_12      -0.1160601000
_diffrn_orient_matrix_UB_13      0.0374832000
_diffrn_orient_matrix_UB_21      0.0948130000
_diffrn_orient_matrix_UB_22      0.0531847000
_diffrn_orient_matrix_UB_23      -0.0178452000
_diffrn_orient_matrix_UB_31      -0.0184292000
_diffrn_orient_matrix_UB_32      0.0009517000
_diffrn_orient_matrix_UB_33      0.1000504000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33145
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.498
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         3.663
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.094
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       prism
_exptl_crystal_F_000             953
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8254
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.4142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7999
_reflns_number_total             8254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02075g2.cif
_cod_data_source_block           fm736
_cod_database_code               7708410
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H59 N5 S3 O1 Cl4 Cu1'
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.602
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O2-O2A
 0.8 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O2 \\sim O2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3. Others
 Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(O2A)=Sof(H2AA)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(O2)=Sof(H2)=FVAR(1)
 Fixed Sof: H5A(0.5) H4A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), N3(H3A,H3B), N4(H4A,H4B), C11(H11A,H11B), C35(H35A,H35B), C2(H2A,
 H2B), C12(H12A,H12B), C26(H26A,H26B), C36(H36A,H36B), C23(H23A,H23B), C13(H13A,
 H13B), C27(H27A,H27B), C14(H14A,H14B), C3(H3C,H3D), C1(H1A,H1B), C25(H25A,
 H25B), C22(H22A,H22B), C15(H15A,H15B), C24(H24A,H24B), C34(H34A,H34B),
 C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C5(H5), C7(H7), C30(H30), C19(H19), C18(H18), C21(H21), C9(H9),
 C17(H17), C31(H31), C6(H6), C33(H33)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C38(H38D,H38E,H38F)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O2A(H2AA)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24711
_shelx_fab_checksum              34373
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.146
_oxdiff_exptl_absorpt_empirical_full_min 0.855