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_7705641
_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 Dy0.091 N O7 Y0.909'
_chemical_formula_sum            'C66 H76 Dy0.09 N O7 Y0.91'
_chemical_formula_weight         1090.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 99.867(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5954(4)
_cell_length_b                   23.3723(7)
_cell_length_c                   20.4784(6)
_cell_measurement_reflns_used    18204
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      28.7410
_cell_measurement_theta_min      3.0900
_cell_volume                     5939.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.886
_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    -41.00 -16.00   0.50    9.89    --    7.10 -37.00-166.00   50
  2  \w      6.00  31.00   0.50    9.89    --    7.10  37.00 -10.00   50
  3  \w    -55.00 -30.00   0.50    9.89    --   -7.50 -37.00-166.00   50
  4  \w     -8.00  17.00   0.50    9.89    --   -7.50  37.00 -10.00   50
  5  \w     50.00  93.00   0.50    9.89    --    7.10  77.00   0.00   86
  6  \w     19.00  92.00   0.50    9.89    --    7.10  57.00 -30.00  146
  7  \w     67.00  94.00   0.50    9.89    --    7.10  77.00 150.00   54
  8  \w     50.00  75.00   0.50    9.89    --    7.10  77.00-120.00   50
  9  \w     51.00  90.00   0.50    9.89    --    7.10  77.00-150.00   78
 10  \w     50.00  93.00   0.50    9.89    --    7.10  77.00  60.00   86
 11  \w    -49.00  -1.00   0.50    9.89    --   -7.50 -77.00 120.00   96
 12  \w    -37.00  36.00   0.50    9.89    --   -7.50  57.00  60.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0125534000
_diffrn_orient_matrix_UB_12      -0.0002841000
_diffrn_orient_matrix_UB_13      0.0351279000
_diffrn_orient_matrix_UB_21      0.0491443000
_diffrn_orient_matrix_UB_22      0.0144078000
_diffrn_orient_matrix_UB_23      -0.0013429000
_diffrn_orient_matrix_UB_31      -0.0263109000
_diffrn_orient_matrix_UB_32      0.0267078000
_diffrn_orient_matrix_UB_33      0.0011297000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72075
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.991
_diffrn_reflns_theta_min         2.529
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             2306
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         13977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0154P)^2^+10.7323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9527
_reflns_number_total             13977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03054f2.cif
_cod_data_source_block           aj0764
_cod_depositor_comments
'Adding full bibliography for 7705640--7705643.cif.'
_cod_database_code               7705641
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H20N1DyYO6
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.778
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Shared sites
{Dy1, Y1}
3. Uiso/Uaniso restraints and constraints
Uanis(Dy1) = Uanis(Y1)
4. Others
 Sof(Y1)=1-FVAR(1)
 Sof(Dy1)=FVAR(1)
5.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)
5.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              62984
_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 7.886
_oxdiff_exptl_absorpt_empirical_full_min 0.417