Comparisons of Lanthanide / Actinide +2 Ions in a Tris(aryloxide)arene Coordination Environment
Fieser, Megan E.; Palumbo, Chad T.; La Pierre, Henry Storms; Halter, Dominik P.; Voora, Vamsee K.; Ziller, Joseph W.; Furche, Filipp; Meyer, Karsten; Evans, William J.; Chem. Sci.  (2017) –; doi:10.1039/C7SC02337E

data_1546972
_publ_section_title
;
 Comparisons of Lanthanide / Actinide +2 Ions in a Tris(aryloxide)arene
 Coordination Environment
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02337E
_journal_year                    2017
_chemical_formula_sum            'C91 H131.5 Dy K O13'
_chemical_formula_weight         1635.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-19 deposited with the CCDC.
2017-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7362(14)
_cell_length_b                   30.6130(19)
_cell_length_c                   25.4472(16)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.28
_cell_volume                     16932.8(19)
_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 0.997
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            170974
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.744
_diffrn_reflns_theta_min         1.149
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             6932
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.718
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         16156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0573P)^2^+47.6570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12496
_reflns_number_total             16156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02337e2.cif
_cod_data_source_block           ctp71
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C91 H131.50 Dy K O13'
_cod_database_code               1546972
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.884
_shelx_res_checksum              8514
_shelx_fab_checksum              15835