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_1557089
_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            'C78 H190 Dy2 K2 N6 O21 Si12'
_chemical_formula_weight         2288.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 103.1276(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.4899(16)
_cell_length_b                   18.8304(12)
_cell_length_c                   25.7453(16)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.31
_cell_volume                     12034.4(13)
_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      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_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  0.0735
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            74183
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.158
_diffrn_reflns_theta_min         1.357
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  0.4319
_exptl_absorpt_correction_T_min  0.3949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       Sphere
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         15305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10683
_reflns_number_total             15305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05794c3.cif
_cod_data_source_block           ajr15
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1557089--1557101.cif.

 Adding full bibliography for 1557089--1557101.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1557089
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.932
_exptl_absorpt_special_details
; 
Reflections not merged 
   75398 Corrected reflections written to file ajr15s.hkl 
 Estimated minimum and maximum transmission:  0.3949  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              70359