#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:43:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179303 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/00/4320064.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320064
loop_
_publ_author_name
'J. Cámpora'
'J. A. López'
'P. Palma'
'D. del Rio'
'E. Carmona'
'P. Valerga'
'C. Graiff'
'A. Tiripicchio'
_publ_section_title
;
 Synthesis and Insertion Reactions of the Cyclometalated Palladium-Alkyl
 Complexes Pd(CH2CMe2-o-C6H4)L2. Observation of a Pentacoordinated
 Intermediate in the Insertion of SO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4116
_journal_page_last               4126
_journal_paper_doi               10.1021/ic010114r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C18 H24 Pd'
_chemical_formula_weight         346.77
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.908(5)
_cell_length_b                   10.311(4)
_cell_length_c                   14.735(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_volume                     3024.7(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Siemens AED'
_diffrn_measurement_method       'θ/2θ 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4458
_diffrn_reflns_theta_full        30.18
_diffrn_reflns_theta_max         30.18
_diffrn_reflns_theta_min         3.16
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_refine_diff_density_max         1.028
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0887P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                2982
_reflns_number_total             4458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010114r_2.cif
_cod_data_source_block           r241f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320064
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.84621(14) 0.0536(3) 0.7060(2) 0.0398(6) Uani 1 d . . .
C2 C 0.83250(16) 0.0458(3) 0.7981(2) 0.0488(7) Uani 1 d . . .
H2 H 0.8414 0.1168 0.8351 0.065(6) Uiso 1 calc R . .
C3 C 0.80593(18) -0.0655(4) 0.8357(3) 0.0560(9) Uani 1 d . . .
H3 H 0.7979 -0.0695 0.8978 0.065(6) Uiso 1 calc R . .
C4 C 0.79132(18) -0.1706(4) 0.7818(3) 0.0566(9) Uani 1 d . . .
H4 H 0.7727 -0.2449 0.8072 0.065(6) Uiso 1 calc R . .
C5 C 0.80421(15) -0.1656(3) 0.6908(3) 0.0493(7) Uani 1 d . . .
H5 H 0.7942 -0.2369 0.6546 0.065(6) Uiso 1 calc R . .
C6 C 0.83214(13) -0.0551(3) 0.6517(2) 0.0390(6) Uani 1 d . . .
C7 C 0.85179(16) -0.0428(3) 0.5538(2) 0.0430(6) Uani 1 d . . .
C8 C 0.8079(2) -0.1198(4) 0.4894(3) 0.0661(10) Uani 1 d . . .
H8A H 0.8235 -0.1077 0.4283 0.080(8) Uiso 1 calc R . .
H8B H 0.7623 -0.0903 0.4943 0.080(8) Uiso 1 calc R . .
H8C H 0.8101 -0.2101 0.5049 0.080(8) Uiso 1 calc R . .
C9 C 0.92445(18) -0.0899(4) 0.5439(3) 0.0596(9) Uani 1 d . . .
H9A H 0.9380 -0.0830 0.4815 0.061(6) Uiso 1 calc R . .
H9B H 0.9275 -0.1788 0.5629 0.061(6) Uiso 1 calc R . .
H9C H 0.9534 -0.0375 0.5809 0.061(6) Uiso 1 calc R . .
C10 C 0.84904(19) 0.1026(3) 0.5343(2) 0.0499(7) Uani 1 d . . .
H10A H 0.8030 0.1274 0.5217 0.054(7) Uiso 1 calc R . .
H10B H 0.8756 0.1213 0.4807 0.054(7) Uiso 1 calc R . .
C11 C 0.8962(2) 0.3607(4) 0.7573(3) 0.0592(9) Uani 1 d . . .
H11 H 0.8596 0.3239 0.7869 0.072(7) Uiso 1 calc R . .
C12 C 0.9532(2) 0.2905(4) 0.7532(3) 0.0607(10) Uani 1 d . . .
H12 H 0.9528 0.2133 0.7859 0.072(7) Uiso 1 calc R . .
C13 C 1.0177(2) 0.3193(6) 0.7031(4) 0.0932(17) Uani 1 d . . .
H13A H 1.0443 0.3766 0.7410 0.142(10) Uiso 1 calc R . .
H13B H 1.0424 0.2387 0.6976 0.142(10) Uiso 1 calc R . .
C14 C 1.0138(2) 0.3772(5) 0.6134(3) 0.0774(13) Uani 1 d . . .
H14A H 1.0542 0.3540 0.5805 0.142(10) Uiso 1 calc R . .
H14B H 1.0139 0.4707 0.6205 0.142(10) Uiso 1 calc R . .
C15 C 0.95476(19) 0.3411(4) 0.5564(2) 0.0547(8) Uani 1 d . . .
H15 H 0.9606 0.2742 0.5148 0.072(7) Uiso 1 calc R . .
C16 C 0.8939(2) 0.3973(4) 0.5600(3) 0.0573(9) Uani 1 d . . .
H16 H 0.8621 0.3664 0.5191 0.072(7) Uiso 1 calc R . .
C17 C 0.8711(3) 0.5035(5) 0.6220(4) 0.0864(16) Uani 1 d . . .
H17A H 0.8897 0.5842 0.5994 0.142(10) Uiso 1 calc R . .
H17B H 0.8227 0.5100 0.6167 0.142(10) Uiso 1 calc R . .
C18 C 0.8870(3) 0.4949(4) 0.7173(4) 0.0926(19) Uani 1 d . . .
H18A H 0.8516 0.5380 0.7508 0.142(10) Uiso 1 calc R . .
H18B H 0.9281 0.5433 0.7277 0.142(10) Uiso 1 calc R . .
Pd1 Pd 0.884150(11) 0.20926(2) 0.639947(15) 0.03699(11) Uani 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
C2 C1 C6 118.2(3) . . ?
C2 C1 Pd1 126.2(2) . . ?
C6 C1 Pd1 115.7(2) . . ?
C3 C2 C1 121.1(3) . . ?
C4 C3 C2 120.3(3) . . ?
C5 C4 C3 119.8(3) . . ?
C4 C5 C6 120.8(3) . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 C7 124.8(3) . . ?
C1 C6 C7 115.4(3) . . ?
C6 C7 C8 114.1(3) . . ?
C6 C7 C10 104.7(3) . . ?
C8 C7 C10 112.1(3) . . ?
C6 C7 C9 108.2(3) . . ?
C8 C7 C9 108.6(3) . . ?
C10 C7 C9 109.1(3) . . ?
C7 C10 Pd1 112.0(2) . . ?
C12 C11 C18 125.0(4) . . ?
C12 C11 Pd1 72.2(2) . . ?
C18 C11 Pd1 108.0(3) . . ?
C11 C12 C13 129.2(4) . . ?
C11 C12 Pd1 74.1(2) . . ?
C13 C12 Pd1 102.9(3) . . ?
C14 C13 C12 118.7(4) . . ?
C13 C14 C15 116.9(4) . . ?
C16 C15 C14 125.5(4) . . ?
C16 C15 Pd1 71.6(2) . . ?
C14 C15 Pd1 109.0(3) . . ?
C15 C16 C17 127.8(4) . . ?
C15 C16 Pd1 74.4(2) . . ?
C17 C16 Pd1 106.4(3) . . ?
C18 C17 C16 118.9(4) . . ?
C17 C18 C11 117.5(4) . . ?
C1 Pd1 C10 79.08(13) . . ?
C1 Pd1 C16 162.97(13) . . ?
C10 Pd1 C16 95.39(14) . . ?
C1 Pd1 C15 161.81(13) . . ?
C10 Pd1 C15 96.86(14) . . ?
C16 Pd1 C15 34.07(13) . . ?
C1 Pd1 C12 99.30(13) . . ?
C10 Pd1 C12 162.11(15) . . ?
C16 Pd1 C12 90.82(15) . . ?
C15 Pd1 C12 79.06(14) . . ?
C1 Pd1 C11 102.24(13) . . ?
C10 Pd1 C11 164.25(15) . . ?
C16 Pd1 C11 78.78(15) . . ?
C15 Pd1 C11 86.50(14) . . ?
C12 Pd1 C11 33.63(14) . . ?
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
C1 C2 1.386(4) . ?
C1 C6 1.405(4) . ?
C1 Pd1 2.023(3) . ?
C2 C3 1.380(5) . ?
C3 C4 1.375(6) . ?
C4 C5 1.366(5) . ?
C5 C6 1.393(4) . ?
C6 C7 1.500(4) . ?
C7 C8 1.514(5) . ?
C7 C10 1.528(5) . ?
C7 C9 1.533(5) . ?
C10 Pd1 2.030(3) . ?
C11 C12 1.348(6) . ?
C11 C18 1.515(6) . ?
C11 Pd1 2.342(4) . ?
C12 C13 1.511(6) . ?
C12 Pd1 2.319(4) . ?
C13 C14 1.452(7) . ?
C14 C15 1.492(6) . ?
C15 C16 1.344(5) . ?
C15 Pd1 2.311(3) . ?
C16 C17 1.496(6) . ?
C16 Pd1 2.276(4) . ?
C17 C18 1.442(7) . ?
