Efficient synthesis of tetradecafluoro-4-phenylheptan-4-ol by a Cannizzaro-type reaction and application of the alcohol as a bulky Martin ligand variant for a new anti-apicophilic phosphorane.
Jiang, Xin-Dong; Matsukawa, Shiro; Kakuda, Ken-Ichiro; Fukuzaki, Yuta; Zhao, Wei-Li; Li, Lin-Song; Shen, Huai-Bin; Kojima, Satoshi; Yamamoto, Yohsuke; Dalton transactions (Cambridge, England : 2003) 39 (2010) 9823–9829; doi:10.1039/c0dt00539h

data_7030428
_publ_section_title
;
 Efficient synthesis of tetradecafluoro-4-phenylheptan-4-ol by a
 Cannizzaro-type reaction and application of the alcohol as a bulky Martin
 ligand variant for a new anti-apicophilic phosphorane.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9823
_journal_page_last               9829
_journal_paper_doi               10.1039/c0dt00539h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C27 H11 F28 O2 P'
_chemical_formula_weight         930.33
_space_group_IT_number           2
_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                83.8130(10)
_cell_angle_beta                 89.4400(10)
_cell_angle_gamma                84.8670(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4620(2)
_cell_length_b                   10.5790(2)
_cell_length_c                   15.9370(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1579.62(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6994
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.9456
_exptl_absorpt_correction_T_min  0.9199
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1076P)^2^+1.4974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1635
_reflns_number_gt                6536
_reflns_number_total             6994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00539h.txt
_cod_data_source_block           compound5a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
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_cod_database_code               7030428