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_7708411
_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         'C40 H57 N7 Ni S3, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H63 Cl2 N9 Ni O8 S3'
_chemical_formula_weight         1071.82
_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
_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                77.4312(16)
_cell_angle_beta                 87.3570(16)
_cell_angle_gamma                73.3222(16)
_cell_formula_units_Z            2
_cell_length_a                   10.7050(2)
_cell_length_b                   14.4139(3)
_cell_length_c                   17.3426(3)
_cell_measurement_reflns_used    31079
_cell_measurement_temperature    195(130)
_cell_measurement_theta_max      74.6120
_cell_measurement_theta_min      3.6930
_cell_volume                     2501.60(9)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      195(130)
_diffrn_detector_area_resol_mean 10.4409
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45139
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.672
_diffrn_reflns_theta_min         3.276
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         10108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+1.8523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9929
_reflns_number_total             10108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02075g2.cif
_cod_data_source_block           FM731s
_cod_original_cell_volume        2501.60(8)
_cod_database_code               7708411
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3), N4(H4)
1.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)
1.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)
1.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              85021
_olex2_submission_special_instructions 'No special instructions were received'