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_7050587
_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            'C37.13 H34.25 Cl0.25 N3 O5 P Pd'
_chemical_formula_weight         748.66
_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                92.7670(6)
_cell_angle_beta                 105.6230(7)
_cell_angle_gamma                114.9541(5)
_cell_formula_units_Z            4
_cell_length_a                   15.0010(2)
_cell_length_b                   15.7410(2)
_cell_length_c                   18.1390(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3675.01(9)
_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 0.988
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45274
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1533
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         19544
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.089
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                11435
_reflns_number_total             19544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302653a.txt
_cod_data_source_block           compound_2
_cod_original_cell_volume        3675.00(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050587