Rare-earth metal complexes with redox-active formazanate ligands
Jin, Da; Sun, Xiaofei; Hinz, Alexander; Roesky, Peter W.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00456A

data_7709741
_publ_section_title
;
 Rare-earth metal complexes with redox-active formazanate ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00456A
_journal_year                    2022
_chemical_formula_moiety         'C33 H33 Dy N4'
_chemical_formula_sum            'C33 H33 Dy N4'
_chemical_formula_weight         648.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2022-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.62(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.179(2)
_cell_length_b                   11.509(2)
_cell_length_c                   12.716(3)
_cell_measurement_reflns_used    42320
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      1.67
_cell_volume                     1411.7(6)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
 394 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23042
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.848
_diffrn_reflns_theta_min         1.690
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.675
_exptl_absorpt_correction_T_max  0.5329
_exptl_absorpt_correction_T_min  0.2423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.194
_refine_diff_density_max         2.531
_refine_diff_density_min         -3.059
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Flack x determined using 2983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1046P)^2^+1.7769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1421
_reflns_d_resolution_high        0.721
_reflns_d_resolution_low         12.192
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.923
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                7090
_reflns_number_total             7733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00456a4.cif
_cod_data_source_block           jd064
_cod_original_cell_volume        1411.6(5)
_cod_database_code               7709741
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.339
_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
 C5-C8A \\sim C5-C8B
 with sigma of 0.02
 C9A-C10A \\sim C10B-C11B
 with sigma of 0.04
 C9A-C11A \\sim C10B-C9B
 with sigma of 0.04
 C10A-C11A \\sim C11B-C9B
 with sigma of 0.04
 C5-C9A \\sim C5-C10B
 with sigma of 0.04
 C5-C10A \\sim C5-C11B
 with sigma of 0.04
 C5-C11A \\sim C5-C9B
 with sigma of 0.04
 C8A-C9A \\sim C8B-C10B
 with sigma of 0.04
 C8A-C10A \\sim C8B-C11B
 with sigma of 0.04
 C8A-C11A \\sim C8B-C9B
 with sigma of 0.04
3. Rigid bond restraints
 C8A, C8B, C9A, C9B, C10A, C10B, C11A, C11B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C8A \\sim C8B \\sim C9A \\sim C9B \\sim C10A \\sim C10B \\sim C11A \\sim C11B:
within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2.5A
5. Others
 Sof(C8B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
6.b Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C10A(H10A,H10B,H10C), C10B(H10D,
 H10E,H10F), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F)
;
_shelx_res_checksum              44457
_shelx_hkl_checksum              67289
_olex2_submission_special_instructions 'No special instructions were received'