A New Class of Functionalized Terpyridyl Ligands as Building Blocks for Photosensitized Supramolecular Architectures. Synthesis, Structural, and Electronic Characterizations
Philippe Lainé; Fethi Bedioui; Philippe Ochsenbein; Valérie Marvaud; Michel Bonin; Edmond Amouyal; Journal of the American Chemical Society 124 (2002) 1364–1377; doi:10.1021/ja011069p

data_4114612
_publ_section_title
;
 A New Class of Functionalized Terpyridyl Ligands as Building Blocks for
 Photosensitized Supramolecular Architectures. Synthesis, Structural, and
 Electronic Characterizations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1364
_journal_page_last               1377
_journal_paper_doi               10.1021/ja011069p
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C38 H27 N4, B F4, 0.5(CH3CO2C2H5)'
_chemical_formula_sum            'C40.5 H27 B F4 N4 O'
_chemical_formula_weight         672.47
_chemical_name_common            H3TP+-tpy
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                116.59(3)
_cell_angle_beta                 105.55(3)
_cell_angle_gamma                93.46(3)
_cell_formula_units_Z            2
_cell_length_a                   10.446(2)
_cell_length_b                   13.750(2)
_cell_length_c                   14.169(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.34
_cell_measurement_theta_min      17.78
_cell_volume                     1714.4(9)
_computing_cell_refinement       'CAD4 Express '
_computing_data_collection       'CAD4 Express '
_computing_data_reduction        MolEn
_computing_molecular_graphics    SHELXTL-plus
_computing_publication_material  XL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'Profile fitted 2\q/\w scans'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.064097
_diffrn_orient_matrix_UB_12      -0.007057
_diffrn_orient_matrix_UB_13      -0.042874
_diffrn_orient_matrix_UB_21      0.027512
_diffrn_orient_matrix_UB_22      0.082871
_diffrn_orient_matrix_UB_23      0.037417
_diffrn_orient_matrix_UB_31      0.073897
_diffrn_orient_matrix_UB_32      -0.000786
_diffrn_orient_matrix_UB_33      0.061283
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6370
_diffrn_reflns_theta_max         66.94
_diffrn_reflns_theta_min         3.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       blocks
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0069(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.744
_refine_ls_goodness_of_fit_obs   1.842
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         4953
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.745
_refine_ls_restrained_S_obs      1.829
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_obs          0.0601
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2337
_refine_ls_wR_factor_obs         0.2005
_reflns_number_observed          4196
_reflns_number_total             6103
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja011069p_1.cif
_cod_data_source_block           H3TP+-tpy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1714.4(6)
_cod_original_formula_sum        'C40.50 H27 B F4 N4 O'
_cod_database_code               4114612