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_4086114
_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            'C50.33 H93.67 Gd K N2 O7.33 Si4'
_chemical_formula_weight         1152.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                116.0433(11)
_cell_angle_beta                 91.3051(12)
_cell_angle_gamma                94.4470(12)
_cell_formula_units_Z            6
_cell_length_a                   11.7545(11)
_cell_length_b                   27.696(3)
_cell_length_c                   30.708(3)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    86(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      2.21
_cell_volume                     8936.9(16)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.9-0, 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 2013/1'
_diffrn_ambient_temperature      86(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_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  0.0784
_diffrn_reflns_av_unetI/netI     0.1169
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            108495
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.291
_diffrn_reflns_theta_min         1.337
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.9958
_exptl_absorpt_correction_T_min  0.7858
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/4'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       plate
_exptl_crystal_F_000             3644
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.296
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1777
_refine_ls_number_reflns         42965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27338
_reflns_number_total             42965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00500_si_012.cif
_cod_data_source_block           ctp4
_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        8936.7(14)
_cod_database_code               4086114
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              24620
_shelx_hkl_checksum              61612