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_1570826
_publ_section_title
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 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            'C46.5 H71 B Ho N9'
_chemical_formula_weight         931.86
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.683(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.814(2)
_cell_length_b                   11.5565(6)
_cell_length_c                   20.0524(10)
_cell_measurement_reflns_used    5418
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.46
_cell_measurement_theta_min      2.312
_cell_volume                     9453.4(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5,SHELXS-13 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.923
_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  0.1243
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68042
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.508
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.054
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6933
_refine_diff_density_max         1.943
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         11080
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0265P)^2^+19.6334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7358
_reflns_number_total             11080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06584g2.cif
_cod_data_source_block           4-Ho_mo_TR114_1_0m
_cod_depositor_comments
'Adding full bibliography for 1570817--1570831.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C46.50 H71 B Ho N9'
_cod_database_code               1570826
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              78251
_shelx_hkl_checksum              51880