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_1546970
_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_absolute_configuration ad
_chemical_formula_sum            'C85 H121.35 Gd K N2 O10'
_chemical_formula_weight         1527.53
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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            4
_cell_length_a                   19.7291(9)
_cell_length_b                   19.7291(9)
_cell_length_c                   19.7291(9)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.31
_cell_volume                     7679.3(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67649
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.016
_diffrn_reflns_theta_min         1.788
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.9263
_exptl_absorpt_correction_T_min  0.8710
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3233
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Flack x determined using 2074 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5062
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0359P)^2^+8.1498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4861
_reflns_number_total             5062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc02337e2.cif
_cod_data_source_block           mef36
_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_cell_volume        7679.3(11)
_cod_database_code               1546970
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.907
_shelx_res_checksum              96606