Solid state conformational and theoretical study of complexes containing the (CxN)Pd moiety (CxN = 2-(phenylazo)phenyl-C,N and its derivatives)
José Pérez; Luis García; Eduardo Pérez; José Luis Serrano; José Francisco Martínez; Gregorio Sánchez; Gregorio López; Arturo Espinosa; Malva Liu; Franciso Sanz; New J. Chem. 27 (2003) 1490–1496; doi:10.1039/b302653a

data_7050586
_publ_section_title
;
 Solid state conformational and theoretical study of complexes
 containing the (CxN)Pd moiety (CxN = 2-(phenylazo)phenyl-C,N and its
 derivatives)
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              1490
_journal_page_last               1496
_journal_paper_doi               10.1039/b302653a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C34 H25 F3 N3 O2 P Pd'
_chemical_formula_weight         701.94
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 101.969(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.628(7)
_cell_length_b                   11.079(3)
_cell_length_c                   17.333(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6129(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.981
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17757
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                4933
_reflns_number_total             8114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302653a.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050586