Ln(II) amido complexes coordinated by ring-expanded N-heterocyclic carbenes - promising catalysts for olefin hydrophosphination.
Lapshin, Ivan V.; Cherkasov, Anton V.; Asachenko, Andrey F.; Trifonov, Alexander A.; Chemical communications (Cambridge, England) 56 (2020) 12913–12916; doi:10.1039/d0cc05424k

data_7127267
_publ_section_title
;
 Ln(II) amido complexes coordinated by ring-expanded N-heterocyclic
 carbenes - promising catalysts for olefin hydrophosphination.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12913
_journal_page_last               12916
_journal_paper_doi               10.1039/d0cc05424k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C34 H64 N4 Si4 Sm'
_chemical_formula_sum            'C34 H64 N4 Si4 Sm'
_chemical_formula_weight         791.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-06 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5699(3)
_cell_length_b                   11.4700(2)
_cell_length_c                   23.5397(5)
_cell_measurement_reflns_used    18825
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9950
_cell_measurement_theta_min      3.3020
_cell_volume                     4190.45(14)
_computing_cell_refinement       'CrysAlis Pro 1.171.38.46'
_computing_data_collection       'CrysAlis Pro 1.171.38.46'
_computing_data_reduction        'CrysAlis Pro 1.171.38.46'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_structure_solution    'SHELXT 2014/5'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku OD Xcalibur (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67548
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.873
_diffrn_reflns_theta_min         3.152
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis Pro 1.171.38.46. Numerical absorption correction based on gaussian
integration over a multifaceted crystal model. Empirical absorption correction
using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       stick
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.830
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0240P)^2^+10.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7856
_reflns_number_total             9885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05424k2.cif
_cod_data_source_block           1_carbsmnsime3
_cod_depositor_comments
'Adding full bibliography for 7127266--7127267.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7127267
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.361
_shelx_estimated_absorpt_t_max   0.825
_shelx_res_checksum              98757