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_7049293
_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 Gd N9 O10, 3(C H4 O)'
_chemical_formula_sum            'C28 H34 Gd N9 O13'
_chemical_formula_weight         861.89
_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             2019-03-04
_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                94.1350(10)
_cell_angle_beta                 104.9910(10)
_cell_angle_gamma                105.1770(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2570(4)
_cell_length_b                   11.7166(4)
_cell_length_c                   13.7355(5)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.21
_cell_volume                     1669.83(10)
_computing_cell_refinement
;
'SAINT V8.35A (?, 2016)'
;
_computing_data_collection
;
'SAINT V8.35A (?, 2016)'
;
_computing_data_reduction
;
'SAINT V8.35A (?, 2016)'
;
_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_temperature      100(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 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25878
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.406
_diffrn_reflns_theta_min         2.566
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.065
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0755 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.8340.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8366
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0353P)^2^+0.5821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6970
_reflns_number_total             8366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00504h2.cif
_cod_data_source_block           mono_gd
_cod_depositor_comments
'Adding full bibliography for 7049290--7049293.cif.'
_cod_database_code               7049293
_shelx_shelxl_version_number     2017/1
_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
 0.87 with sigma of 0.01
 C01C-H3
 1.913106 with sigma of 0.02
 Gd1-H3
 2.929969 with sigma of 0.02
 O0AA-C0AA \\sim O0AB-C0AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O0AA) = Uanis(O0AB)
4. Others
 Sof(H0AE)=Sof(H0AF)=Sof(H0AG)=Sof(O0AB)=Sof(H0AH)=1-FVAR(1)
 Sof(O0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=FVAR(1)
5.a Riding coordinates:
 C0AA(H0AB,H0AC,H0AD), C0AA(H0AE,H0AF,H0AG)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C7(H7), C5(H5A), C24(H24), C12(H12), C17(H17), C19(H19),
 C3(H3A), C14(H14), C15(H15), C2(H2A), C21(H21), C10(H10), C11(H11), C23(H23),
 C9(H9), C22(H22)
5.c Idealised Me refined as rotating group:
 C01C(H01A,H01B,H01C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
5.d Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O8(H8), O0AA(H0AA), O0AB(H0AH)
;
_shelx_res_checksum              14880
_olex2_submission_special_instructions 'No special instructions were received'