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_1570819
_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            'C35 H58 Al B Ho N7'
_chemical_formula_weight         779.60
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   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                81.388(2)
_cell_angle_beta                 80.802(2)
_cell_angle_gamma                66.125(2)
_cell_formula_units_Z            2
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_cell_length_b                   12.0811(8)
_cell_length_c                   15.8693(11)
_cell_measurement_reflns_used    5919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.67
_cell_measurement_theta_min      2.231
_cell_volume                     2040.7(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1017
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43797
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.850
_diffrn_reflns_theta_max         24.850
_diffrn_reflns_theta_min         1.852
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6215
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       needle
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.033
_refine_diff_density_min         -1.650
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     540
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0465P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5377
_reflns_number_total             7013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06584g2.cif
_cod_data_source_block           5-Ho_mo_TR61_2_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 1570817--1570831.cif.'
_cod_database_code               1570819
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.573
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              70749
_shelx_hkl_checksum              66431
_shelx_fab_checksum              60347