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_7717410
_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         'C46 H58 Al Cl Dy F27 O3'
_chemical_formula_sum            'C46 H58 Al Cl Dy F27 O3'
_chemical_formula_weight         1396.85
_chemical_name_systematic        '[Dy(Cpttt)2(Cl)(Al(OC(CF)3)3)3]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2423(2)
_cell_length_b                   14.24450(10)
_cell_length_c                   18.1335(2)
_cell_measurement_reflns_used    21078
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      76.0570
_cell_measurement_theta_min      3.7070
_cell_volume                     5486.94(9)
_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 (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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    106.00 133.00   1.00    1.00    --   43.54  52.00-100.00   27
  2  \w    -20.00  21.00   1.00    1.00    --   43.54  52.00-100.00   41
  3  \w     84.00 109.00   1.00    1.00    --  108.20  52.00-100.00   25
  4  \w     38.00 132.00   1.00    1.00    --   46.06  20.00 -60.00   94
  5  \w     24.00  50.00   1.00    1.00    --   46.06  52.00-100.00   26
  6  \w    -42.00  12.00   1.00    1.00    --   46.06  40.00   0.00   54
  7  \w     12.00 133.00   1.00    1.00    --   46.06  40.00  30.00  121
  8  \w    147.00 198.00   1.00    1.00    --  108.20  50.00   0.00   51
  9  \w     23.00  64.00   1.00    1.00    --  108.20  50.00  30.00   41
 10  \w    148.00 190.00   1.00    1.00    --  108.20  10.00 150.00   42
 11  \w    156.00 197.00   1.00    1.00    --  108.20  50.00  60.00   41
 12  \w    153.00 197.00   1.00    1.00    --  108.20  50.00  30.00   44
 13  \w     92.00 142.00   1.00    1.00    --  108.20  50.00   0.00   50
 14  \w    105.00 131.00   1.00    1.00    --  108.20  50.00  30.00   26
 15  \w     20.00 131.00   1.00    1.00    --  108.20  50.00  60.00  111
 16  \w     45.00 195.00   1.00    1.00    --  108.20   0.00-180.00  150
 17  \w     23.00 192.00   1.00    1.00    --  108.20  50.00 -30.00  169
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0006431000
_diffrn_orient_matrix_UB_12      0.0687560000
_diffrn_orient_matrix_UB_13      -0.0655879000
_diffrn_orient_matrix_UB_21      0.0704458000
_diffrn_orient_matrix_UB_22      0.0204349000
_diffrn_orient_matrix_UB_23      0.0122840000
_diffrn_orient_matrix_UB_31      0.0172818000
_diffrn_orient_matrix_UB_32      -0.0809175000
_diffrn_orient_matrix_UB_33      -0.0525785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38414
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.373
_diffrn_reflns_theta_min         3.736
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    9.090
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.524
_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    1.691
_exptl_crystal_description       block
_exptl_crystal_F_000             2788
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Recrystallised from pentane.'
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.332(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1110
_refine_ls_number_reflns         10820
_refine_ls_number_restraints     3091
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0955P)^2^+9.5039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.893
_reflns_number_gt                10124
_reflns_number_total             10820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02713b2.cif
_cod_data_source_block           ldpm188
_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               7717410
_manchester_internal_diff_code   ldpm188
_manchester_internal_coll_client SCC
_manchester_internal_coll_date   06/02/21
_manchester_internal_process_date 08/02/21
_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         DyClOCFAl
_shelx_estimated_absorpt_t_max   0.454
_shelx_estimated_absorpt_t_min   0.223
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.668(6)
 0.332(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O1A-C35_4 \\sim O1-C35_1 \\sim O2-C35_5 \\sim O2A-C35_2
 with sigma of 0.02
 Al1-O1A \\sim Al1-O1 \\sim Al1-O2 \\sim Al1-O2A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A \\sim Al1 \\sim O1 \\sim O1A \\sim O2 \\sim O3 \\sim F1_1 \\sim
F2_1 \\sim F3_1 \\sim F4_1 \\sim F5_1 \\sim F6_1 \\sim F7_1 \\sim F8_1 \\sim
F9_1 \\sim C35_1 \\sim C36_1 \\sim C37_1 \\sim C38_1 \\sim F1_2 \\sim F2_2
\\sim F3_2 \\sim F4_2 \\sim F5_2 \\sim F6_2 \\sim F7_2 \\sim F8_2 \\sim F9_2
\\sim C35_2 \\sim C36_2 \\sim C37_2 \\sim C38_2 \\sim F1_3 \\sim F2_3 \\sim
F3_3 \\sim F4_3 \\sim F5_3 \\sim F6_3 \\sim F7_3 \\sim F8_3 \\sim F9_3 \\sim
C35_3 \\sim C36_3 \\sim C37_3 \\sim C38_3 \\sim F1_4 \\sim F2_4 \\sim F3_4
\\sim F4_4 \\sim F5_4 \\sim F6_4 \\sim F7_4 \\sim F8_4 \\sim F9_4 \\sim C35_4
\\sim C36_4 \\sim C37_4 \\sim C38_4 \\sim F1_5 \\sim F2_5 \\sim F3_5 \\sim F4_5
\\sim F5_5 \\sim F6_5 \\sim F7_5 \\sim F8_5 \\sim F9_5 \\sim C35_5 \\sim C36_5
\\sim C37_5 \\sim C38_5 \\sim F1_6 \\sim F2_6 \\sim F3_6 \\sim F4_6 \\sim F5_6
\\sim F6_6 \\sim F7_6 \\sim F8_6 \\sim F9_6 \\sim C35_6 \\sim C36_6 \\sim C37_6
\\sim C38_6 \\sim O2A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F1_2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{F1_2, F2_2, F3_2, F4_2, F5_2, F6_2, F7_2, F8_2, F9_2, C35_2, C36_2, C37_2,
C38_2}
{F1_3, F2_3, F3_3, F4_3, F5_3, F6_3, F7_3, F8_3, F9_3, C35_3, C36_3, C37_3,
C38_3}
{F1_4, F2_4, F3_4, F4_4, F5_4, F6_4, F7_4, F8_4, F9_4, C35_4, C36_4, C37_4,
C38_4}
{F1_5, F2_5, F3_5, F4_5, F5_5, F6_5, F7_5, F8_5, F9_5, C35_5, C36_5, C37_5,
C38_5}
{F1_6, F2_6, F3_6, F4_6, F5_6, F6_6, F7_6, F8_6, F9_6, C35_6, C36_6, C37_6,
C38_6}
as
{F1_1, F2_1, F3_1, F4_1, F5_1, F6_1, F7_1, F8_1, F9_1, C35_1, C36_1, C37_1,
C38_1} sigma for 1-2: 0.02 1-3: 0.04
7. Others
 Sof(Cl1A)=Sof(O1A)=Sof(O2A)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(F1)=Sof(F2)=
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(C35)=Sof(C36)=
 Sof(C37)=Sof(C38)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=
 Sof(F8)=Sof(F9)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=1-FVAR(1)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=Sof(F1)=Sof(F2)=
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(C35)=Sof(C36)=
 Sof(C37)=Sof(C38)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=
 Sof(F8)=Sof(F9)=Sof(C35)=Sof(C36)=Sof(C37)=Sof(C38)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
8.b 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)
;
_shelx_res_checksum              41137
_shelx_hkl_checksum              39344
_olex2_exptl_crystal_mounting_method 'Mounted in fomblin.'
_olex2_submission_original_sample_id ldpm188
_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 2.803
_oxdiff_exptl_absorpt_empirical_full_min 0.712