Structure‒solid-state CPMAS 13C NMR correlation in palladacycle solvates (pseudo-polymorphs) with a transformation from Z′ = 1 to Z′ = 2
Ruiz, José; Rodríguez, Venancio; Cutillas, Natalia; Hoffmann, Anke; Chamayou, Anne-Christine; Kazmierczak, Karolina; Janiak, Christoph; CrystEngComm 10 (2008) 1928–; doi:10.1039/b812012a

data_7202425
_publ_section_title
;
 Structure--solid-state CPMAS 13C NMR correlation in palladacycle
 solvates (pseudo-polymorphs) with a transformation from Z&#x2032; = 1
 to Z&#x2032; = 2
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1928
_journal_paper_doi               10.1039/b812012a
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C33 H37 N3 O2 Pd2, 1.5(C7 H8)'
_chemical_formula_sum            'C43.5 H49 N3 O2 Pd2'
_chemical_formula_weight         858.66
_chemical_name_common
;
Bis((N,N-dimethylbenzylamine-kappaN,kappaC)palladium(ii))(mu-
acetato-kappaO:kappaO') (mu-benzophenone iminato-kappaN:kappaN) .
1.5toluene
;
_chemical_name_systematic
;
Bis{(N,N-dimethylbenzylamine-\kN,\kC)palladium(II)}(\m-acetato-\kO:\kO')
(\m-benzophenone iminato-\kN:\kN) . 1.5toluene
;
_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                82.7420(10)
_cell_angle_beta                 83.1070(10)
_cell_angle_gamma                75.9870(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5075(5)
_cell_length_b                   11.3472(6)
_cell_length_c                   18.5747(10)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.2
_cell_volume                     1920.35(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker 1997)'
_computing_data_reduction        'SAINT (Bruker 1997)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart CCD area diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21096
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.8439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.3412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                7089
_reflns_number_total             7772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812012a.txt
_cod_data_source_block           vrr171cs
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C43.50 H49 N3 O2 Pd2'
_cod_database_code               7202425