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_1570830
_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            'C39.5 H67 B Ga Ho N6'
_chemical_formula_weight         871.45
_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   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                96.149(2)
_cell_angle_beta                 100.699(2)
_cell_angle_gamma                110.456(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8291(10)
_cell_length_b                   13.4472(12)
_cell_length_c                   18.5931(17)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.19
_cell_measurement_theta_min      5.016
_cell_volume                     2222.7(4)
_computing_cell_refinement       SAINT
_computing_data_collection       COSMO
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74018
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         1.645
_exptl_absorpt_coefficient_mu    2.404
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       plate
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.557
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.082
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.6347
_refine_diff_density_max         1.263
_refine_diff_density_min         -4.060
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         13452
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0707P)^2^+7.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11473
_reflns_number_total             13452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06584g2.cif
_cod_data_source_block           1-Ho-Ga_ds151b
_cod_depositor_comments
'Adding full bibliography for 1570817--1570831.cif.'
_cod_original_formula_sum        'C39.50 H67 B Ga Ho N6'
_cod_database_code               1570830
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.348
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              29087
_shelx_hkl_checksum              18759