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_7708408
_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
'C37 H55 Cl Cu2 N5 O S3, Cl, B F4, 2(C H4 O), C2 H3 N'
_chemical_formula_sum            'C41 H66 B Cl2 Cu2 F4 N6 O3 S3'
_chemical_formula_weight         1071.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.53744(19)
_cell_length_b                   17.36252(16)
_cell_length_c                   30.7787(4)
_cell_measurement_reflns_used    30400
_cell_measurement_temperature    99.95(10)
_cell_measurement_theta_max      74.5910
_cell_measurement_theta_min      3.7020
_cell_volume                     9906.33(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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   -119.00 -49.00   1.00    5.00    --  -42.65-161.00 108.00   70
  2  \w   -123.00  -2.00   1.00    5.00    --  -42.65 -19.00 150.00  121
  3  \w   -123.00  -2.00   1.00    5.00    --  -42.65 -19.00-150.00  121
  4  \w     83.00 158.00   1.00   15.00    --  108.66  45.00-180.00   75
  5  \w     32.00 137.00   1.00   15.00    --  108.66 -30.00 -90.00  105
  6  \w     83.00 158.00   1.00   15.00    --  108.66  45.00-120.00   75
  7  \w     26.00 108.00   1.00   15.00    --  108.66 -94.00-180.00   82
  8  \w     83.00 158.00   1.00   15.00    --  108.66  45.00 150.00   75
  9  \w     56.00 158.00   1.00   15.00    --  108.66  15.00 120.00  102
 10  \w     36.00 134.00   1.00   15.00    --  108.66 -45.00 150.00   98
 11  \w    -99.00  -2.00   1.00    5.00    --  -42.65 125.00  60.00   97
 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   0.00  100
 14  \w     83.00 158.00   1.00   15.00    --  108.66  45.00   0.00   75
 15  \w     33.00 141.00   1.00   15.00    --  108.66 -77.00   0.00  108
 16  \w     26.00 108.00   1.00   15.00    --  108.66 -94.00 -60.00   82
 17  \w     80.00 122.00   1.00   15.00    --  108.66  61.00 -90.00   42
 18  \w     80.00 158.00   1.00   15.00    --  108.66  61.00 -60.00   78
;
_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      -0.0231770000
_diffrn_orient_matrix_UB_12      -0.0709684000
_diffrn_orient_matrix_UB_13      0.0266082000
_diffrn_orient_matrix_UB_21      -0.0278961000
_diffrn_orient_matrix_UB_22      -0.0387757000
_diffrn_orient_matrix_UB_23      -0.0417717000
_diffrn_orient_matrix_UB_31      0.0747805000
_diffrn_orient_matrix_UB_32      -0.0364456000
_diffrn_orient_matrix_UB_33      -0.0073459000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            94577
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.719
_diffrn_reflns_theta_min         3.733
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       prism
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10090
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0504P)^2^+9.4979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8606
_reflns_number_total             10090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02075g2.cif
_cod_data_source_block           fm667s
_cod_original_cell_volume        9906.34(19)
_cod_database_code               7708408
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N S Cu B Br F'
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.588
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 Cu2-H1
 2.532506 with sigma of 0.02
 C48-H1
 1.874849 with sigma of 0.02
 C38-O3 \\sim C38-O3A
 with sigma of 0.02
2. Others
 Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(O3A)=Sof(H3AA)=1-FVAR(1)
 Sof(O3)=Sof(H3C)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), 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)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C17(H17), C18(H18), C20(H20), C21(H21),
 C29(H29), C30(H30), C32(H32), C33(H33)
3.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C38(H38A,H38B,
 H38C), C38(H38D,H38E,H38F)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2C), O3(H3C), O3A(H3AA)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 72 electrons were 
found in a volume of 264\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per Asymmetric Unit 
which account for 80 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37154
_shelx_fab_checksum              34106
_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 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.783