Rare-earth-metal half-sandwich complexes incorporating methyl, methylidene, and hydrido ligands.
Buschmann, Dennis A.; Schumacher, Lion; Anwander, Reiner; Chemical communications (Cambridge, England) 58 (2022) 9132–9135; doi:10.1039/d2cc03532d

data_7130669
_publ_section_title
;
 Rare-earth-metal half-sandwich complexes incorporating methyl,
 methylidene, and hydrido ligands.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9132
_journal_page_last               9135
_journal_paper_doi               10.1039/d2cc03532d
_journal_volume                  58
_journal_year                    2022
_chemical_formula_sum            'C46 H81 Dy3 O3'
_chemical_formula_weight         1169.60
_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
;
2022-06-23 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                97.942(2)
_cell_angle_beta                 91.931(2)
_cell_angle_gamma                114.983(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3103(7)
_cell_length_b                   11.9001(7)
_cell_length_c                   21.1333(12)
_cell_measurement_reflns_used    1064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.354
_cell_volume                     2540.1(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-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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0930
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51818
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.634
_diffrn_reflns_theta_max         24.634
_diffrn_reflns_theta_min         1.915
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   0.7451
_exptl_transmission_factor_min   0.5482
_refine_diff_density_max         2.269
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8536
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0177P)^2^+3.4016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6815
_reflns_number_total             8536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03532d2.cif
_cod_data_source_block           LS4_0m_a_sq
_cod_database_code               7130669
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.672
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              82403
_shelx_hkl_checksum              63341
_shelx_fab_checksum              60749