 
data_00mau002
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C12 H18 Cl2 N6 O6 Pd'
_chemical_formula_weight          519.62
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'  -0.9988   1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    7.1328(14)
_cell_length_b                    20.699(4)
_cell_length_c                    7.1455(14)
_cell_angle_alpha                 90.00
_cell_angle_beta                  116.17(3)
_cell_angle_gamma                 90.00
_cell_volume                      946.8(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     11269
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.823
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              520
_exptl_absorpt_coefficient_mu     1.305
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD'
_diffrn_measurement_method        'Φ & ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             10091
_diffrn_reflns_av_R_equivalents   0.0487
_diffrn_reflns_av_sigmaI/netI     0.0324
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -26
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        8
_diffrn_reflns_theta_min          3.33
_diffrn_reflns_theta_max          27.51
_reflns_number_total              2165
_reflns_number_gt                 1872
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0239P)²+1.1052P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0048(7)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2165
_refine_ls_number_parameters      161
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0298
_refine_ls_R_factor_gt            0.0229
_refine_ls_wR_factor_ref          0.0572
_refine_ls_wR_factor_gt           0.0538
_refine_ls_goodness_of_fit_ref    0.959
_refine_ls_restrained_S_all       0.959
_refine_ls_shift/su_max           0.561
_refine_ls_shift/su_mean          0.150
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C6 C 0.4612(4) 0.57005(13) 0.8387(4) 0.0270(5) Uani 1 1 d . . .
H4A H 0.540(4) 0.6694(12) 1.079(4) 0.020(6) Uiso 1 1 d . . .
H6C H 0.561(5) 0.5643(14) 0.981(5) 0.042(8) Uiso 1 1 d . . .
H5A H 0.575(4) 0.6817(11) 1.419(4) 0.017(6) Uiso 1 1 d . . .
H6B H 0.437(5) 0.5309(15) 0.775(5) 0.039(8) Uiso 1 1 d . . .
H5B H 0.341(4) 0.6748(12) 1.342(4) 0.025(7) Uiso 1 1 d . . .
H4B H 0.399(4) 0.7245(12) 1.079(4) 0.022(6) Uiso 1 1 d . . .
H3 H -0.210(4) 0.6027(12) 0.654(4) 0.024(6) Uiso 1 1 d . . .
H6A H 0.523(5) 0.5999(15) 0.780(5) 0.047(9) Uiso 1 1 d . . .
H3O H 0.385(5) 0.5793(13) 1.331(4) 0.026(8) Uiso 1 1 d . . .
Pd1 Pd 0.0000 0.5000 0.5000 0.01295(9) Uani 1 2 d S . .
Cl1 Cl 0.01034(9) 0.56856(3) 0.25178(8) 0.02635(14) Uani 1 1 d . . .
N2 N 0.2469(3) 0.64771(8) 0.9351(3) 0.0168(4) Uani 1 1 d . . .
O3 O 0.4822(3) 0.59252(8) 1.3464(3) 0.0266(4) Uani 1 1 d . . .
N3 N 0.0745(3) 0.57347(8) 0.7032(3) 0.0163(3) Uani 1 1 d . . .
O1 O -0.2450(3) 0.70772(8) 0.8674(3) 0.0349(4) Uani 1 1 d . . .
N1 N -0.0537(3) 0.70726(9) 0.9393(3) 0.0256(4) Uani 1 1 d . . .
C2 C 0.2637(3) 0.59626(10) 0.8278(3) 0.0170(4) Uani 1 1 d . . .
C1 C 0.0358(3) 0.65631(9) 0.8731(3) 0.0169(4) Uani 1 1 d . . .
C3 C -0.0685(3) 0.61044(10) 0.7299(3) 0.0168(4) Uani 1 1 d . . .
C5 C 0.4511(4) 0.66030(11) 1.3169(3) 0.0234(5) Uani 1 1 d . . .
C4 C 0.4258(4) 0.68046(11) 1.1031(3) 0.0228(5) Uani 1 1 d . . .
O2 O 0.0613(3) 0.74779(9) 1.0610(3) 0.0443(5) Uani 1 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
C6 0.0156(11) 0.0326(13) 0.0308(13) -0.0088(11) 0.0084(10) -0.0019(10)
Pd1 0.01186(12) 0.01506(13) 0.01121(12) -0.00149(7) 0.00443(8) -0.00234(8)
Cl1 0.0292(3) 0.0292(3) 0.0193(2) 0.0058(2) 0.0095(2) -0.0074(2)
N2 0.0176(8) 0.0173(8) 0.0129(8) -0.0011(6) 0.0042(7) -0.0032(7)
O3 0.0210(9) 0.0249(9) 0.0275(9) 0.0029(7) 0.0048(7) -0.0033(7)
N3 0.0157(8) 0.0165(8) 0.0146(8) -0.0008(6) 0.0049(7) -0.0021(7)
O1 0.0314(10) 0.0337(9) 0.0422(10) -0.0005(8) 0.0187(8) 0.0126(8)
N1 0.0337(11) 0.0195(10) 0.0223(9) -0.0002(7) 0.0113(8) 0.0065(8)
C2 0.0168(10) 0.0189(10) 0.0142(9) -0.0008(8) 0.0060(8) -0.0031(8)
C1 0.0207(10) 0.0152(9) 0.0156(9) 0.0018(7) 0.0087(8) 0.0029(8)
C3 0.0138(9) 0.0198(10) 0.0157(9) 0.0012(8) 0.0055(8) 0.0011(8)
C5 0.0228(11) 0.0236(11) 0.0187(10) -0.0049(8) 0.0045(9) -0.0048(9)
C4 0.0226(11) 0.0212(11) 0.0212(10) -0.0050(8) 0.0064(9) -0.0097(9)
O2 0.0474(12) 0.0307(10) 0.0428(11) -0.0191(8) 0.0092(9) 0.0059(9)
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C6 C2 1.479(3) . ?
Pd1 N3 2.0054(17) . ?
Pd1 N3 2.0054(17) 3_566 ?
Pd1 Cl1 2.2980(6) . ?
Pd1 Cl1 2.2980(6) 3_566 ?
N2 C2 1.348(3) . ?
N2 C1 1.381(3) . ?
N2 C4 1.475(3) . ?
O3 C5 1.421(3) . ?
N3 C2 1.333(3) . ?
N3 C3 1.355(3) . ?
O1 N1 1.228(3) . ?
N1 O2 1.226(3) . ?
N1 C1 1.418(3) . ?
C1 C3 1.353(3) . ?
C5 C4 1.516(3) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N3 Pd1 N3 180.00(6) . 3_566 ?
N3 Pd1 Cl1 90.11(5) . . ?
N3 Pd1 Cl1 89.89(5) 3_566 . ?
N3 Pd1 Cl1 89.89(5) . 3_566 ?
N3 Pd1 Cl1 90.11(5) 3_566 3_566 ?
Cl1 Pd1 Cl1 180.00(2) . 3_566 ?
C2 N2 C1 106.09(16) . . ?
C2 N2 C4 124.32(18) . . ?
C1 N2 C4 129.13(18) . . ?
C2 N3 C3 108.04(17) . . ?
C2 N3 Pd1 128.23(14) . . ?
C3 N3 Pd1 123.70(14) . . ?
O2 N1 O1 124.3(2) . . ?
O2 N1 C1 119.1(2) . . ?
O1 N1 C1 116.56(19) . . ?
N3 C2 N2 109.98(18) . . ?
N3 C2 C6 124.46(19) . . ?
N2 C2 C6 125.53(19) . . ?
C3 C1 N2 108.10(18) . . ?
C3 C1 N1 126.6(2) . . ?
N2 C1 N1 125.22(18) . . ?
C1 C3 N3 107.80(18) . . ?
O3 C5 C4 111.27(19) . . ?
N2 C4 C5 111.67(18) . . ?
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              27.51
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.786
_refine_diff_density_min   -0.716
_refine_diff_density_rms    0.080
