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_7709739
_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         'C57 H45 N12 Y'
_chemical_formula_sum            'C57 H45 N12 Y'
_chemical_formula_weight         986.96
_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             2021-11-04
_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                97.320(3)
_cell_angle_beta                 91.965(3)
_cell_angle_gamma                116.855(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7048(6)
_cell_length_b                   13.1743(5)
_cell_length_c                   15.8425(7)
_cell_measurement_reflns_used    22215
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      1.76
_cell_volume                     2333.74(19)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24348
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.264
_diffrn_reflns_theta_min         1.755
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.7358
_exptl_absorpt_correction_T_min  0.5319
_exptl_absorpt_correction_type   numerical
_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    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9750
_reflns_number_total             12535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00456a4.cif
_cod_data_source_block           jd01-2
_cod_original_cell_volume        2333.74(18)
_cod_database_code               7709739
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.630
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C47(H47), C51(H51), C5(H5), C39(H39), C29(H29), C57(H57), C11(H11), C38(H38),
 C17(H17), C21(H21), C8(H8), C12(H12), C18(H18), C33(H33), C19(H19), C6(H6),
 C13(H13), C48(H48), C27(H27), C37(H37), C23(H23), C41(H41), C53(H53), C9(H9),
 C15(H15), C24(H24), C35(H35), C20(H20), C45(H45), C43(H43), C50(H50), C26(H26),
  C42(H42), C14(H14), C49(H49), C30(H30), C25(H25), C36(H36), C56(H56), C7(H7),
 C54(H54), C44(H44), C31(H31), C32(H32), C55(H55)
;
_shelx_res_checksum              32026
_shelx_hkl_checksum              97780
_olex2_submission_special_instructions 'No special instructions were received'