Study of new metallomacrocyclic Pd(ii) complexes based on hybrid pyrazole sulfoxide/sulfone ligands and their contribution to supramolecular networks
de León, Antonio; Guerrero, Miguel; García-Antón, Jordi; Ros, Josep; Font-Bardía, Mercè; Pons, Josefina; CrystEngComm 15 (2013) 1762–; doi:10.1039/c2ce26687c

data_7209150
_publ_section_title
;
 Study of new metallomacrocyclic Pd(ii) complexes based on hybrid pyrazole
 sulfoxide/sulfone ligands and their contribution to supramolecular
 networks
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1762
_journal_paper_doi               10.1039/c2ce26687c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C28 H44 Cl4 N8 O4 Pd2 S2, 2(H2O)'
_chemical_formula_sum            'C28 H48 Cl4 N8 O6 Pd2 S2'
_chemical_formula_weight         1011.46
_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-97
_cell_angle_alpha                72.55(3)
_cell_angle_beta                 83.78(4)
_cell_angle_gamma                72.72(4)
_cell_formula_units_Z            1
_cell_length_a                   8.186(5)
_cell_length_b                   9.317(4)
_cell_length_c                   13.956(6)
_cell_measurement_reflns_used    81
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     969.4(9)
_computing_cell_refinement       AUTOMAR
_computing_data_collection       MARXDS
_computing_data_reduction        MARSCALE
_computing_molecular_graphics    'ORTEP (Brueggermann and Smith, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device_type  'MAR345 with image plate detector'
_diffrn_measurement_method       'phi scan'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6989
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.93
_diffrn_reflns_theta_min         2.61
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.029(3)
_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_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0884P)^2^+0.7339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                3552
_reflns_number_total             4048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26687c.txt
_cod_data_source_block           film70a
_cod_original_cell_volume        969.4(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7209150