Exploiting complementary ligands for the construction of square antiprismatic monometallic lanthanide SMMs.
Jiao, Yushu; Sarwar, Sidra; Sanz, Sergio; van Leusen, Jan; Izarova, Natalya V.; Campbell, Cameron L.; Brechin, Euan K.; Dalgarno, Scott J.; Kögerler, Paul; Dalton transactions (Cambridge, England : 2003) 50 (2021) 9648–9654; doi:10.1039/d1dt00359c

data_7707705
_publ_section_title
;
 Exploiting complementary ligands for the construction of square
 antiprismatic monometallic lanthanide SMMs.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9648
_journal_page_last               9654
_journal_paper_doi               10.1039/d1dt00359c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C56 H72 Dy O8, C2 H3 N, C16 H36 N'
_chemical_formula_sum            'C74 H111 Dy N2 O8'
_chemical_formula_weight         1319.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.3390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8297(6)
_cell_length_b                   16.0808(4)
_cell_length_c                   21.0550(5)
_cell_measurement_reflns_used    9254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.77
_cell_volume                     6963.4(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex III (Bruker)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            95871
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.110
_diffrn_reflns_theta_min         2.770
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0370 before and 0.0322 after correction.
The Ratio of minimum to maximum transmission is 0.9073.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2796
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.490(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         15176
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0144
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0393
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                14735
_reflns_number_total             15176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt00359c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7707703--7707706.cif.'
_cod_original_cell_volume        6963.3(3)
_cod_database_code               7707705
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.661
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.510(6)
 0.490(6)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C59(H59A,H59B),
 C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
  C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C71(H71A,H71B), C72(H72A,
 H72B), C73(H73A,H73B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C9(H9), C11(H11), C16(H16), C18(H18), C23(H23), C25(H25),
 C49(H49), C54(H54)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C62(H62A,H62B,H62C), C66(H66A,H66B,H66C), C70(H70A,H70B,H70C),
 C74(H74A,H74B,H74C)
;
_shelx_res_checksum              17842
_shelx_hkl_checksum              2466
_olex2_submission_original_sample_id TBC4OMe2DyAcac
_olex2_submission_special_instructions 'No special instructions were received'