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_1557097
_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 Gd K N3 O12 Si6'
_chemical_formula_weight         1206.15
_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                 104.0069(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1493(11)
_cell_length_b                   27.059(3)
_cell_length_c                   21.755(2)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.96
_cell_measurement_theta_min      2.31
_cell_volume                     6368.1(11)
_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 0.943
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78726
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.134
_diffrn_reflns_theta_min         1.223
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.4319
_exptl_absorpt_correction_T_min  0.3744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.009
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         16163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0197P)^2^+17.1322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13374
_reflns_number_total             16163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05794c3.cif
_cod_data_source_block           ajr40
_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               1557097
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.793
_exptl_absorpt_special_details
; 
Reflections not merged 
79704 Corrected reflections written to file ajr40s.hkl 
Estimated minimum and maximum transmission:  0.3744  0.4319 
The ratio of these values is more reliable than their absolute values! 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              13877