Heterometallic Potassium Rare-Earth-Metal Allyl and Hydrido Complexes Stabilized by a Dianionic (NNNN)-Type Macrocyclic Ancillary Ligand
Cui, Peng; Spaniol, Thomas P.; Okuda, Jun; Organometallics 32 (2013) 1176–; doi:10.1021/om300986w

data_4080186
_publ_section_title
;
 Heterometallic Potassium Rare-Earth-Metal Allyl and Hydrido Complexes
 Stabilized by a Dianionic (NNNN)-Type Macrocyclic Ancillary Ligand
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1176
_journal_paper_doi               10.1021/om300986w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C56 H126 K2 N16 O4 Y4'
_chemical_formula_sum            'C56 H126 K2 N16 O4 Y4'
_chemical_formula_weight         1521.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.590(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.997(2)
_cell_length_b                   12.200(2)
_cell_length_c                   18.525(4)
_cell_measurement_reflns_used    4412
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.33
_cell_measurement_theta_min      2.22
_cell_volume                     3574.8(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1128
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41485
_diffrn_reflns_theta_full        26.57
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    3.383
_exptl_absorpt_correction_T_max  0.5811
_exptl_absorpt_correction_T_min  0.4733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.319
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7375
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.3319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                5060
_reflns_number_total             7375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300986w_si_002.cif
_cod_data_source_block           3a
_cod_database_code               4080186