Equilibria between Metallosupramolecular Squares and Triangles with the New Rigid Linker 1,4-Bis(4-pyridyl)tetrafluorobenzene. Experimental and Theoretical Study of the Structural Dependence of NMR Data
Montserrat Ferrer; Mounia Mounir; Oriol Rossell; Eliseo Ruiz; Miguel Angel Maestro; Inorganic Chemistry 42 (2003) 5890–5899; doi:10.1021/ic034489j

data_4314277
_publ_section_title
;
 Equilibria between Metallosupramolecular Squares and Triangles with the
 New Rigid Linker 1,4-Bis(4-pyridyl)tetrafluorobenzene. Experimental and
 Theoretical Study of the Structural Dependence of NMR Data
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5890
_journal_page_last               5899
_journal_paper_doi               10.1021/ic034489j
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C36 H32 F6 Fe O8 P2 Pd S2'
_chemical_formula_weight         994.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.67(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2828(11)
_cell_length_b                   18.0154(16)
_cell_length_c                   18.1363(16)
_cell_measurement_temperature    298(2)
_cell_volume                     3977.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22956
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  0.9380
_exptl_absorpt_correction_T_min  0.7666
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         8093
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+5.1624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1896
_reflns_number_gt                4931
_reflns_number_total             8093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034489jsi20030509_124917_2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+5.1624P] 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^)+(0.1006P)^2^+5.1624P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4314277