Mononuclear lanthanide complexes assembled from a tridentate NNO donor ligand: design of a Dy<sup>III</sup> single-ion magnet.
Kalita, Pankaj; Malakar, Amit; Goura, Joydeb; Nayak, Subhashree; Herrera, Juan Manuel; Colacio, Enrique; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4857–4866; doi:10.1039/c9dt00504h

data_7049291
_publ_section_title
;
 Mononuclear lanthanide complexes assembled from a tridentate NNO donor
 ligand: design of a Dy<sup>III</sup> single-ion magnet.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4857
_journal_page_last               4866
_journal_paper_doi               10.1039/c9dt00504h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C25 H22 N9 O10 Tb, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 N9 O13 Tb'
_chemical_formula_weight         863.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-04 deposited with the CCDC.    2019-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                93.856(2)
_cell_angle_beta                 105.196(3)
_cell_angle_gamma                105.168(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3219(3)
_cell_length_b                   11.7730(3)
_cell_length_c                   13.7532(4)
_cell_measurement_reflns_used    18921
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      29.1300
_cell_measurement_theta_min      2.8920
_cell_volume                     1689.22(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.874
_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    -35.00  -9.00   0.50    1.85    --    7.20 -66.00 157.00   52
  2  \w     33.00  59.00   0.50    1.85    --    7.20  66.00 -67.00   52
  3  \w    -42.00   3.00   0.50    1.85    --   -7.60 -66.00 157.00   90
  4  \w     -4.00  21.00   0.50    1.85    --   -7.60  66.00 -67.00   50
  5  \w    -80.00  13.00   0.50    1.85    --    7.20 -57.00   0.00  186
  6  \w    -23.00  45.00   0.50    1.85    --    7.20  57.00 -30.00  136
  7  \w    -22.00  82.00   0.50    1.85    --    7.20  57.00 120.00  208
  8  \w     50.00  97.00   0.50    1.85    --    7.20  77.00-150.00   94
  9  \w     63.00  94.00   0.50    1.85    --    7.20  77.00 -90.00   62
 10  \w    -58.00 -23.00   0.50    1.85    --   -7.60 -82.00 -90.00   70
 11  \w    -43.00 -18.00   0.50    1.85    --   -7.60 -82.00  90.00   50
 12  \w    -16.00   9.00   0.50    1.85    --   -7.60 -82.00 -90.00   50
 13  \w    -57.00  29.00   0.50    1.85    --   -7.60 -82.00   0.00  172
;
_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      0.0074087000
_diffrn_orient_matrix_UB_12      -0.0464768000
_diffrn_orient_matrix_UB_13      0.0291549000
_diffrn_orient_matrix_UB_21      0.0622087000
_diffrn_orient_matrix_UB_22      0.0354356000
_diffrn_orient_matrix_UB_23      0.0284682000
_diffrn_orient_matrix_UB_31      -0.0260142000
_diffrn_orient_matrix_UB_32      0.0237800000
_diffrn_orient_matrix_UB_33      0.0354638000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.994
_diffrn_reflns_theta_min         2.821
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42732
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7845
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+1.2759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7199
_reflns_number_total             7845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00504h2.cif
_cod_data_source_block           aj0805
_cod_depositor_comments
'Adding full bibliography for 7049290--7049293.cif.'
_cod_database_code               7049291
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNOTb
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.683
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C25-H3
 1.893253 with sigma of 0.02
 Tb1-H3
 2.932969 with sigma of 0.02
 O0AA-C0AA \\sim O1A-C0AA
 with sigma of 0.02
 C0AA-O0AA \\sim O0AA-O1A
 with sigma of 0.02
3. Others
 Sof(H0AE)=Sof(H0AF)=Sof(H0AG)=Sof(O1A)=Sof(H1A)=1-FVAR(1)
 Sof(O0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C19(H19), N5(H5), C3(H3A), C12(H12), C24(H24), C5(H5A), C17(H17),
 C7(H7), C23(H23), C15(H15), C11(H11), C10(H10), C22(H22), C2(H2A), C9(H9),
 C21(H21), C14(H14)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C01E(H01A,H01B,H01C), C01G(H01D,H01E,H01F), C0AA(H0AB,
 H0AC,H0AD), C0AA(H0AE,H0AF,H0AG)
4.c Idealised tetrahedral OH refined as rotating group:
 O00I(H00I), O00O(H00O), O0AA(H0AA), O1A(H1A)
;
_shelx_res_checksum              29513
_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 2.093
_oxdiff_exptl_absorpt_empirical_full_min 0.628