A cascade reaction: ring-opening insertion of dioxaphospholane into lutetium alkyl bonds.
Johnson, Kevin R. D.; Hayes, Paul G.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2448–2457; doi:10.1039/c3dt52790e

data_7028792
_publ_section_title
;
 A cascade reaction: ring-opening insertion of dioxaphospholane into
 lutetium alkyl bonds.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2448
_journal_page_last               2457
_journal_paper_doi               10.1039/c3dt52790e
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C88 H124 Lu2 N6 O8 P4 Si4'
_chemical_formula_weight         1980.11
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                80.777(4)
_cell_angle_beta                 84.329(4)
_cell_angle_gamma                83.766(4)
_cell_formula_units_Z            2
_cell_length_a                   14.763(5)
_cell_length_b                   18.123(6)
_cell_length_c                   19.174(6)
_cell_measurement_reflns_used    6423
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.51
_cell_measurement_theta_min      2.20
_cell_volume                     5016(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0818
_diffrn_reflns_av_sigmaI/netI    0.1081
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54488
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    2.119
_exptl_absorpt_correction_T_max  0.9334
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
One heavily disordered pentane solvent molecule was present
in the asymmetric unit, for which no suitable model could be found. 
The electron density associated with the disordered regions was 
removed from the reflection file using SQUEEZE (Platon), leaving a 
void of ca. 510.0 A^3.
;
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         20429
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                13249
_reflns_number_total             20429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52790e.txt
_cod_data_source_block           Compound8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028792