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_7709743
_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 N4 Yb'
_chemical_formula_sum            'C33 H33 N4 Yb'
_chemical_formula_weight         658.67
_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    32486
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.46
_cell_measurement_theta_min      2.12
_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      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 529 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'single reflection optic'
_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  0.0733
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12584
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.111
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_type              'Xenocs Genix3D microfocus'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.341
_exptl_absorpt_correction_T_max  0.7106
_exptl_absorpt_correction_T_min  0.3431
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.061
_refine_diff_density_max         4.548
_refine_diff_density_min         -3.326
_refine_diff_density_rms         0.277
_refine_ls_abs_structure_details
;
 Flack x determined using 2244 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5536
_refine_ls_number_restraints     655
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0841
_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^)+(0.1026P)^2^+33.3020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2154
_reflns_d_resolution_high        0.679
_reflns_d_resolution_low         9.612
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                5320
_reflns_number_total             5536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00456a4.cif
_cod_data_source_block           jd057bt
_cod_original_cell_volume        1411.6(5)
_cod_database_code               7709743
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.461
_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. Rigid bond restraints
 C11, C25, C12, C7, C2, C24, C26, C9, C17, C33, C28, C31, C27, C22, C8, C13,
 C16, C20, C3, C18, C10, C1, C29, N3, C15, N2, N1, N4, Yb, C6, C14, C21, C30,
 C4, C5, C32, C23, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim C25 \\sim C12 \\sim C7 \\sim C2 \\sim C24 \\sim C26 \\sim C9 \\sim
C17 \\sim C33 \\sim C28 \\sim C31 \\sim C27 \\sim C22 \\sim C8 \\sim C13 \\sim
C16 \\sim C20 \\sim C3 \\sim C18 \\sim C10 \\sim C1 \\sim C29 \\sim N3 \\sim
C15 \\sim N2 \\sim N1 \\sim N4 \\sim Yb \\sim C6 \\sim C14 \\sim C21 \\sim C30
\\sim C4 \\sim C5 \\sim C32 \\sim C23 \\sim C19: within 2.5A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2.5A
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C31(H31), C4(H4), C32(H32), C21(H21), C23(H23), C33(H33), C13(H13),
 C30(H30), C14(H14), C20(H20), C19(H19), C3(H3), C16(H16), C29(H29), C15(H15),
 C22(H22), C17(H17), C7(H7), C28(H28), C24(H24), C26(H26), C27(H27), C25(H25)
4.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              54523
_shelx_hkl_checksum              66694
_olex2_submission_special_instructions 'No special instructions were received'