Terminal dysprosium and holmium organoimides.
Rieser, Theresa E.; Schädle, Dorothea; Maichle-Mössmer, Cäcilia; Anwander, Reiner; Chemical science 15 (2024) 3562–3570; doi:10.1039/d3sc06584g

data_1570820
_publ_section_title
;
 Terminal dysprosium and holmium organoimides.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              3562
_journal_page_last               3570
_journal_paper_doi               10.1039/d3sc06584g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C55 H91 B N9 O3 Y'
_chemical_formula_weight         1026.08
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_method           SHELXL-2019/3
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.928(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4785(19)
_cell_length_b                   17.511(3)
_cell_length_c                   14.619(2)
_cell_measurement_reflns_used    8598
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      2.321
_cell_volume                     2825.6(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'APEX3 v2019.11-0'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1234
_diffrn_reflns_av_unetI/netI     0.1073
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34654
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        22.520
_diffrn_reflns_theta_max         22.520
_diffrn_reflns_theta_min         1.449
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            farblos
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.072
_exptl_transmission_factor_max   0.7447
_exptl_transmission_factor_min   0.5348
_refine_diff_density_max         1.067
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 2238 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.098(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         7276
_refine_ls_number_restraints     1973
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0971
_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^)+(0.0564P)^2^+25.2506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                6237
_reflns_number_total             7276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06584g2.cif
_cod_data_source_block           4-Y-mo_TR180_0m_a
_cod_depositor_comments
'Adding full bibliography for 1570817--1570831.cif.'
_cod_original_cell_volume        2825.5(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1570820
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              66003
_shelx_hkl_checksum              56856