Lanthanide Complexes of the Kläui Metalloligand, CpCo(P=O(OR)2)3: An Examination of Ligand Exchange Kinetics between Isotopomers by Electrospray Mass Spectrometry
Kevin J. H. Allen; Emma C. Nicholls-Allison; Kevin R. D. Johnson; Rajinder S. Nirwan; David J. Berg; Dennis Wester; Brendan Twamley; Inorganic Chemistry 51 (2012) 12436–12443; doi:10.1021/ic301830u

data_4331081
_publ_section_title
;
 Lanthanide Complexes of the Kl\"aui Metalloligand, CpCo(P=O(OR)2)3: An
 Examination of Ligand Exchange Kinetics between Isotopomers by
 Electrospray Mass Spectrometry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12436
_journal_page_last               12443
_journal_paper_doi               10.1021/ic301830u
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C82 H70 Co2 O18 P6 Yb, 2(C6 H6), C4 H8 Cl3 Co O'
_chemical_formula_sum            'C98 H90 Cl3 Co3 O19 P6 Yb'
_chemical_formula_weight         2213.70
_chemical_name_common            '[(Klaui)2Yb][CoCl3.THF] + 2C6H6'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6632(7)
_cell_length_b                   19.7358(7)
_cell_length_c                   24.5563(9)
_cell_measurement_reflns_used    7125
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.21
_cell_volume                     9529.5(6)
_computing_cell_refinement       'Bruker, 2006; SAINT+  v. 7.23a'
_computing_data_collection       'Bruker, 2006; SMART v. 5.632'
_computing_data_reduction        'Bruker, 2006; SAINT+  v. 7.23a'
_computing_molecular_graphics    'Bruker, 2003; XP, SHELXTL  v. 6.14'
_computing_publication_material  'Bruker, 2001; XCIF, SHELXTL, v. 6.14'
_computing_structure_refinement  'Bruker, 2003; XL,SHELXTL  v. 6.14''
_computing_structure_solution    'Bruker, 2003; XS, SHELXTL  v. 6.14'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            123863
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.739
_exptl_absorpt_correction_T_max  0.9181
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 ; Bruker, 2004'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       needle
_exptl_crystal_F_000             4488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         17278
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+5.3510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                14363
_reflns_number_total             17278
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301830u_si_003.cif
_cod_data_source_block           bt1005
_cod_database_code               4331081