New palladium and platinum polyfluorophenyl complexes with pyrazolyl N-donor ligands. Analysis of the restricted rotation of the polyfluorophenyl rings
Carmen Carrión, M.; Díaz, Alberto; Guerrero, Ana; Jalón, Félix A.; Manzano, Blanca R.; Rodríguez, Ana; New Journal of Chemistry 26 (2002) 305–; doi:10.1039/b108139j

data_7050709
_publ_section_title
;
 New palladium and platinum polyfluorophenyl complexes with pyrazolyl
 N-donor ligands. Analysis of the restricted rotation of the
 polyfluorophenyl rings
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              305
_journal_paper_doi               10.1039/b108139j
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C33 H24 F10 Fe N4 Pd'
_chemical_formula_weight         828.81
_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                 105.41(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8040(10)
_cell_length_b                   16.86(3)
_cell_length_c                   15.137(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3150(6)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7576
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.122
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                4494
_reflns_number_total             7576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b108139j.txt
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7050709