Isolation of +2 rare earth metal ions with three anionic carbocyclic rings: bimetallic bis(cyclopentadienyl) reduced arene complexes of La2+and Ce2+are four electron reductants
Kotyk, Christopher M.; Fieser, Megan E.; Palumbo, Chad T.; Ziller, Joseph W.; Darago, Lucy E.; Long, Jeffrey R.; Furche, Filipp; Evans, William J.; Chem. Sci. 6 (2015) 7267–; doi:10.1039/C5SC02486B

data_1540648
_publ_section_title
;
 Isolation of +2 rare earth metal ions with three anionic carbocyclic
 rings: bimetallic bis(cyclopentadienyl) reduced arene complexes of
 La2+and Ce2+are four electron reductants
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              7267
_journal_paper_doi               10.1039/C5SC02486B
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C81 H141 K2 La2 N4 O13 Si4'
_chemical_formula_weight         1847.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-30 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.3261(11)
_cell_length_b                   54.668(3)
_cell_length_c                   16.5827(9)
_cell_measurement_reflns_used    9461
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.38
_cell_volume                     18426.5(17)
_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      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            194473
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.069
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             7736
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.077
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         18865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+105.8975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16255
_reflns_number_total             18865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02486b2.cif
_cod_data_source_block           cmk26
_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 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               1540648
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              11709