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_7709745
_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         'C69 H69 N12 Yb, 1.5(C5 H12)'
_chemical_formula_sum            'C76.5 H87 N12 Yb'
_chemical_formula_weight         1347.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-16 deposited with the CCDC.	2022-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                81.535(7)
_cell_angle_beta                 80.353(7)
_cell_angle_gamma                69.971(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4474(10)
_cell_length_b                   15.2412(10)
_cell_length_c                   19.8619(19)
_cell_measurement_reflns_used    42746
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      1.68
_cell_volume                     3473.7(5)
_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 (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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
 914 frames, detector distance = 100 mm
;
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40102
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.527
_diffrn_reflns_theta_min         1.686
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  0.8051
_exptl_absorpt_correction_T_min  0.5979
_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_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.484
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         19290
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15029
_reflns_number_total             19290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00456a4.cif
_cod_data_source_block           jd070
_cod_original_formula_sum        'C76.50 H87 N12 Yb'
_cod_database_code               7709745
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1A-C1B = C1B-C1C = C1C-C1D = C1D-C1E
 1.52 with sigma of 0.02
 C1A-C1C = C1B-C1D = C1C-C1E
 2.54 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D \\sim C1D-C1E
 with sigma of 0.02
 C1A-C1C \\sim C1C-C1E \\sim C1B-C1D
 with sigma of 0.04
3. Rigid bond restraints
 C1A, C1B, C1C, C1D, C1E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E: within 2.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C9AA) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.012
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) H1BA(0.5)
 H1BB(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) C1E(0.5)
 H1EA(0.5) H1EB(0.5) H1EC(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C6AA(H6AA,H6AB), C7AA(H7AA,H7AB), C8AA(H8AA,H8AB), C1B(H1BA,H1BB), C1C(H1CA,
 H1CB), C1D(H1DA,H1DB)
7.b Aromatic/amide H refined with riding coordinates:
 C68(H68), C67(H67), C66(H66), C28(H28), C25(H25), C69(H69), C23(H23),
 C45(H45), C63(H63), C22(H22), C16(H16), C21(H21), C61(H61), C46(H46), C47(H47),
  C59(H59), C15(H15), C37(H37), C17(H17), C24(H24), C18(H18), C31(H31),
 C65(H65), C62(H62), C5(H5), C40(H40), C60(H60), C6(H6), C38(H38), C41(H41),
 C30(H30), C50(H50), C9(H9), C39(H39), C19(H19), C44(H44), C43(H43), C8(H8),
 C27(H27), C49(H49), C52(H52), C53(H53)
7.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C56(H56A,H56B,H56C), C13(H13A,H13B,
 H13C), C11(H11A,H11B,H11C), C55(H55A,H55B,H55C), C9AA(H9AA,H9AB,H9AC),
 C0BA(H0BA,H0BB,H0BC), C12(H12A,H12B,H12C), C33(H33A,H33B,H33C), C57(H57A,H57B,
 H57C), C1A(H1AA,H1AB,H1AC), C1E(H1EA,H1EB,H1EC)
;
_shelx_res_checksum              52493
_shelx_hkl_checksum              84458
_olex2_submission_special_instructions 'No special instructions were received'