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_1570824
_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            'C43 H68 Al B Ho N7'
_chemical_formula_weight         885.76
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-12-05 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5531(9)
_cell_length_b                   11.2886(5)
_cell_length_c                   19.1515(8)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.486
_cell_volume                     4430.4(3)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35460
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.770
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       column
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.4878
_exptl_transmission_factor_min   0.4086
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 4778 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         11130
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                10539
_reflns_number_total             11130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06584g2.cif
_cod_data_source_block           mo_TR90c_0m_b
_cod_depositor_comments
'Adding full bibliography for 1570817--1570831.cif.'
_cod_original_cell_volume        4430.3(3)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1570824
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.633
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              92063
_shelx_hkl_checksum              99145