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_7202424
_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, 0.5 (C12 H12), 0.5(C6 H6)'
_chemical_formula_sum            'C42 H46 N3 O2 Pd2'
_chemical_formula_weight         837.62
_chemical_name_common
;
Bis((N,N-dimethylbenzylamine-kappaN,kappaC)palladium(ii))(mu-
acetato-kappaO:kappaO') (mu-benzophenone iminato-kappaN:kappaN) .
1.5benzene
;
_chemical_name_systematic
;
Bis{(N,N-dimethylbenzylamine-\kN,\kC)palladium(II)}(\m-acetato-\kO:\kO')
(\m-benzophenone iminato-\kN:\kN) . 1.5benzene
;
_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                83.304(3)
_cell_angle_beta                 84.253(3)
_cell_angle_gamma                78.682(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3712(5)
_cell_length_b                   11.2535(7)
_cell_length_c                   18.6983(11)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      31.36
_cell_measurement_theta_min      2.25
_cell_volume                     1914.31(19)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII AXS CCD 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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30419
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.9500
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                6641
_reflns_number_total             7746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812012a.txt
_cod_data_source_block           c6h6171a
_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_database_code               7202424