Mechanistic insight into the lanthanide (III) salt catalysed monoacylation of symmetrical diols from structural models
Clarke, Paul A.; Arnold, Polly L.; Smith, Martin A.; Natrajan, Louise S.; Wilson, Claire; Chan, Chuen; Chemical Communications (Cambridge, United Kingdom)  (2003) 2588–2589; doi:10.1039/b308171k

data_7113636
_publ_section_title
;
 Mechanistic insight into the lanthanide (III) salt catalysed
 monoacylation of symmetrical diols from structural models
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   20
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2588
_journal_page_last               2589
_journal_paper_doi               10.1039/b308171k
_journal_year                    2003
_chemical_formula_moiety         'C51 H81 O9 Pr'
_chemical_formula_sum            'C51 H81 O9 Pr'
_chemical_formula_weight         979.07
_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
'placed geometrically, except H61 and H62 located from difference map'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.191(7)
_cell_angle_beta                 81.482(6)
_cell_angle_gamma                81.016(5)
_cell_formula_units_Z            2
_cell_length_a                   10.576(3)
_cell_length_b                   12.662(4)
_cell_length_c                   20.988(6)
_cell_measurement_reflns_used    17476
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.3
_cell_volume                     2706.3(14)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'SHELXL-97; enCIFer (CCDC, 2003); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_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  0.055
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39109
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        2.1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.482
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SHELXTL version 6.12; Bruker, 2001)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.08
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment
'riding model, except H61 and H62 (distance restraints applied)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         12439
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                10631
_reflns_number_total             12439
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104852
_cod_data_source_file            b308171k.txt
_cod_data_source_block           PRMHBZ
_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/retrospective/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               7113636