Kinetic and Mechanistic Investigation of Metallacycle Ring Opening in an Ortho-Metalated Lutetium Aryl Complex
Johnson, Kevin R. D.; Hayes, Paul G.; Organometallics 30 (2011) 58–; doi:10.1021/om100814h

data_4063674
_publ_section_title
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 Kinetic and Mechanistic Investigation of Metallacycle Ring Opening in an
 Ortho-Metalated Lutetium Aryl Complex
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_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              58
_journal_paper_doi               10.1021/om100814h
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C74 H81 Lu N4 P2'
_chemical_formula_weight         1263.34
_chemical_name_systematic
;

 ?

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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.0580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.990(3)
_cell_length_b                   23.689(2)
_cell_length_c                   23.446(2)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      2.20
_cell_volume                     17774(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            123715
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: (Sheldrick 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;

Total electron count and void volume indicated that 16 pentane molecules per unit cell were removed from the reflection file by the SQUEEZE routine. In this CIF file, the density and MW calculations refer only to that of the SQUEEZED structure and do not account for the presence of these solvent molecules. Please refer to the article (Table 1) for the adjusted density and MW calculations, where the 16 pentane molecules per unit cell are accounted for.
;
_refine_diff_density_max         2.391
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         19565
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                12319
_reflns_number_total             19565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100814h_si_001.cif
_cod_data_source_block           ph10011
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4063674