Low-coordinate rare-earth complexes of the asymmetric 2,4-di-tert-butylphenolate ligand prepared by redox transmetallation/protolysis reactions, and their reactivity towards ring-opening polymerisation.
Clark, Lawrence; Deacon, Glen B.; Forsyth, Craig M.; Junk, Peter C.; Mountford, Philip; Townley, Josh P.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 6693–6704; doi:10.1039/c0dt00023j

data_7025846
_publ_section_title
;
 Low-coordinate rare-earth complexes of the asymmetric
 2,4-di-tert-butylphenolate ligand prepared by redox
 transmetallation/protolysis reactions, and their reactivity towards
 ring-opening polymerisation.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6693
_journal_page_last               6704
_journal_paper_doi               10.1039/c0dt00023j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C54 H87 O6 Pr'
_chemical_formula_sum            'C54 H87 O6 Pr'
_chemical_formula_weight         973.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.19(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.575(4)
_cell_length_b                   28.185(6)
_cell_length_c                   19.489(4)
_cell_measurement_reflns_used    4377
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.23
_cell_volume                     10736(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO-SMN and Scalepack'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KAPPA CCD'
_diffrn_measurement_method       'thin slice phi and omeg 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  0.1339
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112224
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.616
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         24565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.0597
_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
[0.00000+1.00000exp(0.60(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0805P)^2^+0.0000sin\q/\l]
where P = 0.33330Fo^2^ + 0.66670Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                15392
_reflns_number_total             24565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00023j.txt
_cod_data_source_block           josh02
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7025846