Synthesis and lanthanide coordination chemistry of trifluoromethyl derivatives of phosphinoylmethyl pyridine N-oxides
Pailloux, Sylvie; Shirima, Cornel Edicome; Ray, Alisha D.; Duesler, Eileen N.; Smith, Karen Ann; Paine, Robert T.; Klaehn, John R.; McIlwain, Michael E.; Hay, Benjamin P.; Dalton Transactions  (2009) 7486–7493; doi:10.1039/b905947d

data_7002175
_publ_section_title
;
 Synthesis and lanthanide coordination chemistry of trifluoromethyl
 derivatives of phosphinoylmethyl pyridine N-oxides
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              7486
_journal_page_last               7493
_journal_paper_doi               10.1039/b905947d
_journal_year                    2009
_chemical_formula_moiety         'C20 H14 F6 N O2 P'
_chemical_formula_sum            'C20 H14 F6 N O2 P'
_chemical_formula_weight         445.29
_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                84.198(4)
_cell_angle_beta                 81.657(4)
_cell_angle_gamma                72.516(4)
_cell_formula_units_Z            2
_cell_length_a                   7.8219(6)
_cell_length_b                   8.8196(7)
_cell_length_c                   14.4992(12)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      65.73
_cell_measurement_theta_min      5.47
_cell_volume                     942.18(13)
_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      225(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25744
_diffrn_reflns_theta_full        33.07
_diffrn_reflns_theta_max         33.07
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker,SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0426
_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[\s^2^(Fo^2^)+(0.0573P)^2^+0.4033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                5849
_reflns_number_total             7013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905947d.txt
_cod_data_source_block           rpsl32
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7002175