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_7705642
_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 Er N O7'
_chemical_formula_sum            'C66 H76 Er N O7'
_chemical_formula_weight         1162.53
_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                106.5780(10)
_cell_angle_beta                 94.7510(10)
_cell_angle_gamma                91.3860(10)
_cell_formula_units_Z            4
_cell_length_a                   12.5323(2)
_cell_length_b                   19.8358(3)
_cell_length_c                   25.8063(4)
_cell_measurement_reflns_used    9208
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.51
_cell_volume                     6119.67(17)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            94211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.062
_diffrn_reflns_theta_min         1.072
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0669 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.8921. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1439
_refine_ls_number_reflns         24124
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0367P)^2^+1.0809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17376
_reflns_number_total             24124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03054f2.cif
_cod_data_source_block           vc_pk_419b_er_0m
_cod_depositor_comments
'Adding full bibliography for 7705640--7705643.cif.'
_cod_database_code               7705642
_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. Restrained distances
 Er1B-O7C \\sim Er1B-O7B
 with sigma of 0.02
 N1C-C11C \\sim N1B-C12B
 with sigma of 0.02
 O7B-C10B \\sim O7C-C10C
 with sigma of 0.02
 N1B-C10B \\sim N1C-C10C
 with sigma of 0.02
 N1B-C11B \\sim N1C-C12C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.22A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.22A
4. Rigid body (RIGU) restrains
 O7B, N1B, C10B, C11B, C12B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7C, N1C, C10C, C11C, C12C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O7C)=Sof(N1C)=Sof(C10C)=Sof(H10C)=Sof(C11C)=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C12C)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(O7B)=Sof(N1B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C5A(H5A), C8A(H8A), C10A(H10A), C15A(H15A), C17A(H17A), C21A(H21A),
 C23A(H23A), C27A(H27A), C29A(H29A), C33A(H33A), C35A(H35A), C39A(H39A),
 C41A(H41A), C45A(H45A), C47A(H47A), C2B(H2B), C5B(H5B), C8B(H8B), C10B(H10B),
 C10C(H10C), C15B(H15B), C17B(H17B), C21B(H21B), C23B(H23B), C27B(H27B),
 C29B(H29B), C33B(H33B), C35B(H35B), C39B(H39B), C41B(H41B), C45B(H45B),
 C47B(H47B)
6.b Idealised Me refined as rotating group:
 C11A(H11G,H11H,H11I), C12A(H12G,H12H,H12I), C49A(H49D,H49E,H49F), C50A(H50D,
 H50E,H50F), C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F),
 C54A(H54D,H54E,H54F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F), C57A(H57D,
 H57E,H57F), C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F),
 C61A(H61D,H61E,H61F), C62A(H62D,H62E,H62F), C63A(H63D,H63E,H63F), C64A(H64D,
 H64E,H64F), C65A(H65D,H65E,H65F), C66A(H66D,H66E,H66F), C11B(H11A,H11B,H11C),
 C11C(H11D,H11E,H11F), C12B(H12A,H12B,H12C), C12C(H12D,H12E,H12F), C49B(H49A,
 H49B,H49C), C50B(H50A,H50B,H50C), C51B(H51A,H51B,H51C), C52B(H52A,H52B,H52C),
 C53B(H53A,H53B,H53C), C54B(H54A,H54B,H54C), C55B(H55A,H55B,H55C), C56B(H56A,
 H56B,H56C), C57B(H57A,H57B,H57C), C58B(H58A,H58B,H58C), C59B(H59A,H59B,H59C),
 C60B(H60A,H60B,H60C), C61B(H61A,H61B,H61C), C62B(H62A,H62B,H62C), C63B(H63A,
 H63B,H63C), C64B(H64A,H64B,H64C), C65B(H65A,H65B,H65C), C66B(H66A,H66B,H66C)
;
_shelx_res_checksum              90143
_olex2_submission_special_instructions 'No special instructions were received'