The importance of the counter-cation in reductive rare-earth metal chemistry: 18-crown-6 instead of 2,2,2-cryptand allows isolation of [YII(NR2)3]1− and ynediolate and enediolate complexes from CO reactions
Ryan, Austin J.; Ziller, Joseph W.; Evans, William J.; Chemical Science 11 (2020) 2006–2014; doi:10.1039/C9SC05794C

data_1557100
_publ_section_title
;
 The importance of the counter-cation in reductive rare-earth metal
 chemistry: 18-crown-6 instead of 2,2,2-cryptand allows isolation of
 [YII(NR2)3]1&#x2212; and ynediolate and enediolate complexes from CO
 reactions
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              2006
_journal_page_last               2014
_journal_paper_doi               10.1039/C9SC05794C
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C42 H102 K N3 O12 Si6 Y'
_chemical_formula_weight         1137.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-29 deposited with the CCDC.	2020-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0003(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0774(7)
_cell_length_b                   27.0905(18)
_cell_length_c                   21.7959(14)
_cell_measurement_reflns_used    9025
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.32
_cell_volume                     6346.5(7)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.909
_diffrn_reflns_theta_min         1.221
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       square
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.227
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         15678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0669P)^2^+6.8680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12476
_reflns_number_total             15678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05794c3.cif
_cod_data_source_block           ajr28
_cod_depositor_comments
;Adding full bibliography for 1557089--1557101.cif.

 Adding full bibliography for 1557089--1557101.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1557100
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.691
_shelx_estimated_absorpt_t_max   0.781
_exptl_absorpt_special_details
; 
77263 Corrected reflections written to file ajr28s.hkl 
Estimated minimum and maximum transmission:  0.6480  0.7458 
The ratio of these values is more reliable than their absolute values! 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              45428