Seven-coordinate Ln<sup>III</sup> complexes assembled from a bulky <sup> <i>Mes</i> </sup>acacH ligand: their synthesis, structure, photoluminescence and SMM behaviour.
Kalita, Pankaj; Nayak, Prakash; Ahmed, Naushad; Herrera, Juan Manuel; Venkatasubbaiah, Krishnan; Colacio, Enrique; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15404–15416; doi:10.1039/d0dt03054f

data_7705643
_publ_section_title
;
 Seven-coordinate Ln<sup>III</sup> complexes assembled from a bulky <sup>
 <i>Mes</i> </sup>acacH ligand: their synthesis, structure,
 photoluminescence and SMM behaviour.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15404
_journal_page_last               15416
_journal_paper_doi               10.1039/d0dt03054f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C66 H76 N O7 Tb'
_chemical_formula_sum            'C66 H76 N O7 Tb'
_chemical_formula_weight         1154.19
_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
_audit_creation_date             2020-09-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2020-09-20 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                94.6660(10)
_cell_angle_beta                 99.1700(10)
_cell_angle_gamma                106.0000(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2338(3)
_cell_length_b                   13.8401(3)
_cell_length_c                   19.6751(5)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.48
_cell_volume                     3133.69(13)
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54629
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         1.753
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0687 before and 0.0384 after correction. The Ratio of minimum to maximum transmission is 0.6684. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         19073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0374P)^2^+0.5925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16171
_reflns_number_total             19073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03054f2.cif
_cod_data_source_block           vc_pk_419_tb_0m
_cod_depositor_comments
'Adding full bibliography for 7705640--7705643.cif.'
_cod_database_code               7705643
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C10(H10), C15(H15), C17(H17), C21(H21), C23(H23),
 C27(H27), C29(H29), C33(H33), C35(H35), C39(H39), C41(H41), C45(H45), C47(H47)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              40345
_olex2_submission_special_instructions 'No special instructions were received'