Ligand Effects in the Synthesis of Ln2+Complexes by Reduction of Tris(cyclopentadienyl) Precursors Including C‒H Bond Activation of an Indenyl Anion
Corbey, Jordan F.; Woen, David H.; Palumbo, Chad T.; Fieser, Megan E.; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Organometallics 34 (2015) 3909–; doi:10.1021/acs.organomet.5b00500

data_4086111
_publ_section_title
;
 Ligand Effects in the Synthesis of Ln2+Complexes by Reduction of
 Tris(cyclopentadienyl) Precursors Including C--H Bond Activation of an
 Indenyl Anion
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3909
_journal_paper_doi               10.1021/acs.organomet.5b00500
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C24 H29 Cl2 Dy K O1.5'
_chemical_formula_weight         613.97
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.9116(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.005(3)
_cell_length_b                   7.8383(8)
_cell_length_c                   24.439(3)
_cell_measurement_temperature    143(2)
_cell_volume                     5031.4(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            29873
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.131
_diffrn_reflns_theta_min         1.551
_exptl_absorpt_coefficient_mu    3.363
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.516
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0242P)^2^+9.6193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5328
_reflns_number_total             6442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00500_si_008.cif
_cod_data_source_block           jfc77
_cod_depositor_comments
'Adding full bibliography for 4086111--4086114.cif.'
_cod_original_cell_volume        5031.3(9)
_cod_original_formula_sum        'C24 H29 Cl2 Dy K O1.50'
_cod_database_code               4086111
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.276
_shelx_estimated_absorpt_t_max   0.847
_shelx_res_checksum              33057
_shelx_hkl_checksum              69832