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_7049290
_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 Dy N9 O10, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 Dy N9 O13'
_chemical_formula_weight         867.14
_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     iterative
_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                94.491(2)
_cell_angle_beta                 105.765(2)
_cell_angle_gamma                105.073(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3165(3)
_cell_length_b                   11.6740(4)
_cell_length_c                   13.7042(2)
_cell_measurement_reflns_used    13019
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.9910
_cell_measurement_theta_min      2.9240
_cell_volume                     1660.65(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -53.00   0.00   1.00   21.88    --    3.50 -55.00 122.00   53
  2  \w    -23.00  92.00   1.00   21.88    --    3.50  55.00 -94.00  115
  3  \w    -84.00  33.00   1.00   21.88    --    3.50 -38.00 -30.00  117
  4  \w      6.00  70.00   1.00   21.88    --   -3.80  38.00-150.00   64
  5  \w    -42.00 -10.00   1.00   21.88    --   -3.80 -82.00-180.00   32
  6  \w    -26.00   1.00   1.00   21.88    --   -3.80 -82.00  60.00   27
  7  \w    -62.00  31.00   1.00   21.88    --   -3.80 -82.00  90.00   93
  8  \w    -63.00  35.00   1.00   21.88    --   -3.80 -82.00 -30.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31915
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.566
_exptl_absorpt_coefficient_mu    2.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63614
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       plate
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.737
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+5.6669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6103
_reflns_number_total             6862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00504h2.cif
_cod_data_source_block           aj0023r
_cod_depositor_comments
'Adding full bibliography for 7049290--7049293.cif.'
_cod_original_cell_volume        1660.64(8)
_cod_database_code               7049290
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.542
_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 O(H) groups
2. Restrained distances
 O10-H10
 0.85 with sigma of 0.01
 O13-C28
 1.42 with sigma of 0.002
 C25-H10
 1.907547 with sigma of 0.02
 Dy1-H10
 2.893164 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N2(H2), C24(H24), C19(H19), C15(H15), C12(H12), C5(H5), C6(H6A),
 C3(H3), C7(H7), C17(H17), C9(H9), C21(H21), C18(H18), C22(H22), C23(H23),
 C11(H11), C10(H10A)
4.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C)
4.c Idealised tetrahedral OH refined as rotating group:
 O11(H11A), O13(H13), O12(H12A)
;
_shelx_res_checksum              31291
_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
;