Influence of weakly coordinating anions binding to the hexa-<i>tert</i>-butyl dysprosocenium cation.
Corner, Sophie C.; Gransbury, Gemma K.; Mills, David P.; Dalton transactions (Cambridge, England : 2003) 54 (2024) 198–206; doi:10.1039/d4dt02713b

data_7717411
_publ_section_title
;
 Influence of weakly coordinating anions binding to the
 hexa-<i>tert</i>-butyl dysprosocenium cation.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              198
_journal_page_last               206
_journal_paper_doi               10.1039/d4dt02713b
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C74 H63 Al Cl Dy F30 O2, 2(C6 H5 F)'
_chemical_formula_sum            'C86 H73 Al Cl Dy F32 O2'
_chemical_formula_weight         1971.37
_chemical_name_systematic        '[Dy(Cpttt)2(Cl)(Al(CH2CH3)(OC(C6F5)3)2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                72.902(3)
_cell_angle_beta                 78.936(2)
_cell_angle_gamma                85.763(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3345(3)
_cell_length_b                   16.0941(5)
_cell_length_c                   21.5697(7)
_cell_measurement_reflns_used    13932
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      28.5800
_cell_measurement_theta_min      3.5720
_cell_volume                     4015.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.839
_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    -39.00   4.00   1.00    4.00    --  -17.16 -77.00 -90.00   43
  2  \w     -4.00  29.00   1.00    4.00    --   18.25  37.00 -90.00   33
  3  \w    -36.00  47.00   1.00    4.00    --   18.25 -77.00  30.00   83
  4  \w     -4.00  87.00   1.00    4.00    --   18.25  37.00   0.00   91
  5  \w    -10.00  36.00   1.00    4.00    --   18.25  77.00 150.00   46
  6  \w     39.00  67.00   1.00    4.00    --   18.25 178.00-150.00   28
  7  \w     38.00  89.00   1.00    4.00    --   18.25  37.00 -90.00   51
  8  \w     -8.00  22.00   1.00    4.00    --   18.25  77.00 -90.00   30
  9  \w      4.00  35.00   1.00    4.00    --   18.25 -57.00 120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0061909000
_diffrn_orient_matrix_UB_12      0.0117117000
_diffrn_orient_matrix_UB_13      0.0297425000
_diffrn_orient_matrix_UB_21      0.0069272000
_diffrn_orient_matrix_UB_22      -0.0442428000
_diffrn_orient_matrix_UB_23      0.0176201000
_diffrn_orient_matrix_UB_31      0.0578637000
_diffrn_orient_matrix_UB_32      0.0056803000
_diffrn_orient_matrix_UB_33      -0.0052499000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36237
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.360
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1978
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Recrystallised from fluorobenzene.'
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.167
_refine_diff_density_max         2.423
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1191
_refine_ls_number_reflns         18504
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+15.3033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15087
_reflns_number_total             18504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02713b2.cif
_cod_data_source_block           adpm658
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717410--7717411.cif.
;
_cod_database_code               7717411
_manchester_internal_diff_code   adpm658
_manchester_internal_coll_client SCC
_manchester_internal_coll_date   06/12/20
_manchester_internal_process_date 05/01/21
_manchester_internal_process_user SCC
_manchester_internal_solution_date 19/09/24
_manchester_internal_solution_user SCC
_manchester_internal_refinement_date 19/09/24
_manchester_internal_refinement_user SCC
_manchester_internal_validation_date 19/09/24
_manchester_internal_validation_user SCC
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyAlBO2F30C74H67
_chemical_oxdiff_usercomment     sc74a
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.630
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F32A-C81A \\sim F32-C81
 with sigma of 0.02
 F32-C82 \\sim F32A-C82A \\sim F32-C86 \\sim F32A-C86A
 with sigma of 0.02
 C82-C81 \\sim C82A-C81A \\sim C83A-C82A \\sim C83-C82 \\sim C84A-C83A \\sim
C84-C83 \\sim C85A-C84A ~
 C85-C84 \\sim C86A-C85A \\sim C86-C85 \\sim C86A-C81A \\sim C86-C81
 with sigma of 0.02
 C86-C82 \\sim C85-C81 \\sim C83-C81 \\sim C84-C82 \\sim C85-C83 \\sim C86-C84
\\sim C86A-C82A \\sim C85A-
 C81A \\sim C83A-C81A \\sim C84A-C82A \\sim C85A-C83A \\sim C86A-C84A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F32 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim F32A
\\sim C81A \\sim C82A \\sim C83A \\sim C84A \\sim C85A \\sim C86A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F32, C81, C82, C83, C84, C85, C86, F32A, C81A, C82A, C83A, C84A, C85A, C86A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F32A)=Sof(C81A)=Sof(C82A)=Sof(H82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=
 Sof(H84A)=Sof(C85A)=Sof(H85A)=Sof(C86A)=Sof(H86A)=1-FVAR(1)
 Sof(F32)=Sof(C81)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(H83)=Sof(C84)=Sof(H84)=
 Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C35(H35a,H35b)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22), C76(H76), C77(H77), C78(H78), C79(H79),
 C80(H80), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C82A(H82A),
 C83A(H83A), C84A(H84A), C85A(H85A), C86A(H86A)
6.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c),
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C17(H17a,H17b,H17c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C26(H26a,
 H26b,H26c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c), C30(H30a,H30b,H30c),
 C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c), C36(H36a,H36b,
 H36c)
;
_shelx_res_checksum              86116
_shelx_hkl_checksum              74634
_olex2_exptl_crystal_mounting_method 'Mounted in fomblin.'
_olex2_submission_original_sample_id adpm658
_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 3.401
_oxdiff_exptl_absorpt_empirical_full_min 0.436