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_4086236
_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_absolute_configuration unk
_chemical_formula_sum            'C22 H29 O Y'
_chemical_formula_weight         398.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2717(14)
_cell_length_b                   12.6044(19)
_cell_length_c                   16.250(2)
_cell_measurement_reflns_used    4648
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.51
_cell_volume                     1899.0(5)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      128(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.947
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.706
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_correction_T_min  0.6198
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/2'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.492(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0520P)^2^+0.6188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.769
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.950
_reflns_number_gt                3782
_reflns_number_total             4540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00500_si_010.cif
_cod_data_source_block           dhw4
_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 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4086236
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.767
_shelxl_version_number           2014/6
_shelx_res_checksum              78810
_shelx_hkl_checksum              65006