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_4086113
_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 ad
_chemical_formula_sum            'C31 H29 O Y'
_chemical_formula_weight         506.45
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                120
_cell_formula_units_Z            2
_cell_length_a                   11.6507(11)
_cell_length_b                   11.6507(11)
_cell_length_c                   10.0984(10)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.85
_cell_volume                     1187.1(2)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2013.10-0, 2013'
_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      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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  0.0244
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14058
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.623
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  0.8382
_exptl_absorpt_correction_T_min  0.4380
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/4'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       rod
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.774
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
; 
 Flack x determined using 866 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.018(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+1.1365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.861
_reflns_friedel_fraction_full    0.994
_reflns_friedel_fraction_max     0.935
_reflns_number_gt                1906
_reflns_number_total             1965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00500_si_003.cif
_cod_data_source_block           jfc50
_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 

 Adding full bibliography for 4086111--4086114.cif.
;
_cod_original_cell_volume        1187.1(3)
_cod_database_code               4086113
_shelx_estimated_absorpt_t_min   0.250
_shelx_estimated_absorpt_t_max   0.745
_shelxl_version_number           2014/6
_shelx_res_checksum              19423
_shelx_hkl_checksum              13613