#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:54:59 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178760 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/14/4101481.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_4101481
loop_
_publ_author_name
'Sui-Seng, Christine'
'Enright, Gary D'
'Zargarian, Davit'
_publ_section_title
;
 New palladium(II)-(eta(3/5)- or eta1-indenyl) and
 dipalladium(I)-(mu,eta3-indenyl) complexes.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6508
_journal_page_last               6519
_journal_paper_doi               10.1021/ja060747a
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_sum            'C15 H22 Cl N Pd'
_chemical_formula_weight         358.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 95.3970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.77560(10)
_cell_length_b                   13.9797(2)
_cell_length_c                   12.42090(10)
_cell_measurement_reflns_used    7669
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.84
_cell_measurement_theta_min      3.16
_cell_volume                     1517.04(3)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart 2000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18428
_diffrn_reflns_theta_full        72.91
_diffrn_reflns_theta_max         72.91
_diffrn_reflns_theta_min         4.77
_diffrn_standards_decay_%        -0.02
_diffrn_standards_number         139
_exptl_absorpt_coefficient_mu    11.331
_exptl_absorpt_correction_T_max  0.5600
_exptl_absorpt_correction_T_min  0.1600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.686
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0280
_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/[σ²(Fo²)+(0.0532P)²+0.7659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                2908
_reflns_number_total             3002
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja060747asi20060207_072742.cif
_cod_data_source_block           suse23
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (23
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (55
times).

'_geom_torsion_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (122 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4101481
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'
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
Pd Pd 0.627770(17) 0.168045(10) 0.474567(12) 0.01694(9) Uani 1 1 d .
Cl Cl 0.68692(6) 0.09135(3) 0.31445(4) 0.02430(13) Uani 1 1 d .
N N 0.8466(2) 0.24074(13) 0.49634(15) 0.0181(4) Uani 1 1 d .
C1 C 0.3917(3) 0.12524(16) 0.4687(2) 0.0260(5) Uani 1 1 d .
H1 H 0.3786 0.0698 0.4245 0.031 Uiso 1 1 calc R
C2 C 0.4519(3) 0.12706(16) 0.5774(2) 0.0274(5) Uani 1 1 d .
H2 H 0.4641 0.0736 0.6247 0.033 Uiso 1 1 calc R
C3 C 0.4908(3) 0.22237(16) 0.60351(19) 0.0225(5) Uani 1 1 d .
H3 H 0.5568 0.2430 0.6641 0.027 Uiso 1 1 calc R
C3A C 0.4112(3) 0.28472(16) 0.52054(19) 0.0201(4) Uani 1 1 d .
C4 C 0.3966(3) 0.38307(17) 0.5127(2) 0.0238(5) Uani 1 1 d .
H4 H 0.4344 0.4236 0.5706 0.029 Uiso 1 1 calc R
C5 C 0.3247(3) 0.42096(17) 0.4170(2) 0.0290(5) Uani 1 1 d .
H5 H 0.3115 0.4882 0.4106 0.035 Uiso 1 1 calc R
C6 C 0.2720(3) 0.3626(2) 0.3313(2) 0.0309(6) Uani 1 1 d .
H6 H 0.2265 0.3906 0.2664 0.037 Uiso 1 1 calc R
C7 C 0.2847(3) 0.26299(19) 0.3389(2) 0.0283(5) Uani 1 1 d .
H7 H 0.2482 0.2230 0.2802 0.034 Uiso 1 1 calc R
C7A C 0.3520(3) 0.22425(16) 0.4344(2) 0.0215(5) Uani 1 1 d .
C8 C 0.9734(3) 0.16940(15) 0.5095(2) 0.0227(5) Uani 1 1 d .
H8A H 1.0718 0.2040 0.5232 0.027 Uiso 1 1 calc R
H8B H 0.9761 0.1336 0.4410 0.027 Uiso 1 1 calc R
C9 C 0.9594(3) 0.09851(17) 0.6006(2) 0.0276(5) Uani 1 1 d .
H9A H 0.9620 0.1329 0.6695 0.041 Uiso 1 1 calc R
H9B H 1.0448 0.0531 0.6034 0.041 Uiso 1 1 calc R
H9C H 0.8625 0.0637 0.5879 0.041 Uiso 1 1 calc R
C10 C 0.8471(3) 0.30561(16) 0.59232(18) 0.0208(4) Uani 1 1 d .
H10A H 0.8381 0.2656 0.6572 0.025 Uiso 1 1 calc R
H10B H 0.7547 0.3464 0.5826 0.025 Uiso 1 1 calc R
C11 C 0.9862(3) 0.37069(19) 0.6150(2) 0.0294(5) Uani 1 1 d .
H11A H 1.0799 0.3322 0.6187 0.044 Uiso 1 1 calc R
H11B H 0.9801 0.4038 0.6840 0.044 Uiso 1 1 calc R
H11C H 0.9880 0.4179 0.5568 0.044 Uiso 1 1 calc R
C12 C 0.8679(3) 0.29714(16) 0.39601(18) 0.0207(4) Uani 1 1 d .
H12A H 0.8710 0.2523 0.3346 0.025 Uiso 1 1 calc R
H12B H 0.9679 0.3303 0.4058 0.025 Uiso 1 1 calc R
C13 C 0.7432(3) 0.37083(16) 0.36752(19) 0.0249(5) Uani 1 1 d .
H13A H 0.6428 0.3398 0.3645 0.037 Uiso 1 1 calc R
H13B H 0.7573 0.3992 0.2970 0.037 Uiso 1 1 calc R
H13C H 0.7492 0.4211 0.4228 0.037 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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_publ_flag
C1 PD N 166.93(8) y
C1 PD C2 37.88(10) y
N PD C2 136.16(9) y
C1 PD C3 62.32(9) y
N PD C3 106.42(8) y
C2 PD C3 37.28(9) y
C1 PD CL 97.61(7) y
N PD CL 93.19(5) y
C2 PD CL 126.92(7) y
C3 PD CL 159.79(7) y
C1 PD C7A 35.45(8) y
N PD C7A 133.94(7) y
C2 PD C7A 58.79(8) y
C3 PD C7A 57.87(8) y
CL PD C7A 104.79(6) y
C1 PD C3A 57.46(8) y
N PD C3A 109.57(7) y
C2 PD C3A 57.53(8) y
C3 PD C3A 34.38(8) y
CL PD C3A 133.73(5) y
C7A PD C3A 32.00(7) y
C8 N C10 111.79(18) y
C8 N C12 107.03(17) y
C10 N C12 110.58(17) y
C8 N PD 110.07(13) y
C10 N PD 108.63(13) y
C12 N PD 108.69(13) y
C2 C1 C7A 108.5(2) y
C2 C1 PD 71.83(13) y
C7A C1 PD 87.09(13) y
C2 C1 H1 125.8 ?
C7A C1 H1 125.8 ?
PD C1 H1 108.1 ?
C1 C2 C3 107.5(2) y
C1 C2 PD 70.30(13) y
C3 C2 PD 73.44(13) y
C1 C2 H2 126.2 ?
C3 C2 H2 126.2 ?
PD C2 H2 121.7 ?
C2 C3 C3A 108.1(2) y
C2 C3 PD 69.28(13) y
C3A C3 PD 87.19(14) y
C2 C3 H3 126 ?
C3A C3 H3 126 ?
PD C3 H3 110 ?
C4 C3A C7A 120.8(2) y
C4 C3A C3 132.2(2) y
C7A C3A C3 106.8(2) y
C4 C3A PD 132.11(15) y
C7A C3A PD 71.68(13) y
C3 C3A PD 58.43(12) y
C3A C4 C5 117.9(2) y
C3A C4 H4 121 ?
C5 C4 H4 121 ?
C6 C5 C4 121.4(2) y
C6 C5 H5 119.3 ?
C4 C5 H5 119.3 ?
C5 C6 C7 121.0(2) y
C5 C6 H6 119.5 ?
C7 C6 H6 119.5 ?
C7A C7 C6 118.2(2) y
C7A C7 H7 120.9 ?
C6 C7 H7 120.9 ?
C7 C7A C3A 120.5(2) y
C7 C7A C1 133.0(2) y
C3A C7A C1 106.3(2) y
C7 C7A PD 127.51(17) y
C3A C7A PD 76.32(13) y
C1 C7A PD 57.46(12) y
N C8 C9 114.0(2) y
N C8 H8A 108.8 ?
C9 C8 H8A 108.8 ?
N C8 H8B 108.8 ?
C9 C8 H8B 108.8 ?
H8A C8 H8B 107.6 ?
C8 C9 H9A 109.5 ?
C8 C9 H9B 109.5 ?
H9A C9 H9B 109.5 ?
C8 C9 H9C 109.5 ?
H9A C9 H9C 109.5 ?
H9B C9 H9C 109.5 ?
N C10 C11 116.73(19) y
N C10 H10A 108.1 ?
C11 C10 H10A 108.1 ?
N C10 H10B 108.1 ?
C11 C10 H10B 108.1 ?
H10A C10 H10B 107.3 ?
C10 C11 H11A 109.5 ?
C10 C11 H11B 109.5 ?
H11A C11 H11B 109.5 ?
C10 C11 H11C 109.5 ?
H11A C11 H11C 109.5 ?
H11B C11 H11C 109.5 ?
N C12 C13 113.99(18) y
N C12 H12A 108.8 ?
C13 C12 H12A 108.8 ?
N C12 H12B 108.8 ?
C13 C12 H12B 108.8 ?
H12A C12 H12B 107.6 ?
C12 C13 H13A 109.5 ?
C12 C13 H13B 109.5 ?
H13A C13 H13B 109.5 ?
C12 C13 H13C 109.5 ?
H13A C13 H13C 109.5 ?
H13B C13 H13C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd C1 2.151(2) y
Pd N 2.1674(18) y
Pd C2 2.171(2) y
Pd C3 2.225(2) y
Pd Cl 2.3598(5) y
Pd C7a 2.548(2) y
Pd C3a 2.608(2) y
N C8 1.491(3) y
N C10 1.498(3) y
N C12 1.501(3) y
C1 C2 1.403(4) y
C1 C7a 1.480(3) y
C1 H1 0.95 ?
C2 C3 1.406(3) y
C2 H2 0.95 ?
C3 C3a 1.474(3) y
C3 H3 0.95 ?
C3a C4 1.383(4) y
C3a C7a 1.422(3) y
C4 C5 1.396(3) y
C4 H4 0.95 ?
C5 C6 1.386(4) y
C5 H5 0.95 ?
C6 C7 1.399(4) y
C6 H6 0.95 ?
C7 C7a 1.385(3) y
C7 H7 0.95 ?
C8 C9 1.518(3) y
C8 H8a 0.99 ?
C8 H8b 0.99 ?
C9 H9a 0.98 ?
C9 H9b 0.98 ?
C9 H9c 0.98 ?
C10 C11 1.527(3) y
C10 H10a 0.99 ?
C10 H10b 0.99 ?
C11 H11a 0.98 ?
C11 H11b 0.98 ?
C11 H11c 0.98 ?
C12 C13 1.520(3) y
C12 H12a 0.99 ?
C12 H12b 0.99 ?
C13 H13a 0.98 ?
C13 H13b 0.98 ?
C13 H13c 0.98 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
C1 PD N C8 153.1(3) y
C2 PD N C8 96.68(17) y
C3 PD N C8 123.72(15) y
CL PD N C8 -61.24(14) y
C7A PD N C8 -175.36(14) y
C3A PD N C8 159.78(14) y
C1 PD N C10 30.3(4) y
C2 PD N C10 -26.02(18) y
C3 PD N C10 1.02(15) y
CL PD N C10 176.06(13) y
C7A PD N C10 61.93(17) y
C3A PD N C10 37.07(15) y
C1 PD N C12 -90.0(4) y
C2 PD N C12 -146.40(13) y
C3 PD N C12 -119.36(14) y
CL PD N C12 55.69(13) y
C7A PD N C12 -58.44(16) y
C3A PD N C12 -83.30(14) y
N PD C1 C2 -69.9(4) y
C3 PD C1 C2 -37.90(13) y
CL PD C1 C2 144.63(12) y
C7A PD C1 C2 -110.51(19) y
C3A PD C1 C2 -77.47(14) y
N PD C1 C7A 40.6(4) y
C2 PD C1 C7A 110.51(19) y
C3 PD C1 C7A 72.61(14) y
CL PD C1 C7A -104.86(13) y
C3A PD C1 C7A 33.04(13) y
C7A C1 C2 C3 -15.9(2) y
PD C1 C2 C3 64.51(15) y
C7A C1 C2 PD -80.45(16) y
N PD C2 C1 162.14(12) y
C3 PD C2 C1 116.1(2) y
CL PD C2 C1 -45.87(15) y
C7A PD C2 C1 39.43(13) y
C3A PD C2 C1 77.27(14) y
C1 PD C2 C3 -116.1(2) y
N PD C2 C3 46.05(19) y
CL PD C2 C3 -161.96(11) y
C7A PD C2 C3 -76.66(14) y
C3A PD C2 C3 -38.82(13) y
C1 C2 C3 C3A 17.3(2) y
PD C2 C3 C3A 79.73(16) y
C1 C2 C3 PD -62.44(15) y
C1 PD C3 C2 38.51(15) y
N PD C3 C2 -148.68(14) y
CL PD C3 C2 45.8(2) y
C7A PD C3 C2 79.32(15) y
C3A PD C3 C2 110.5(2) y
C1 PD C3 C3A -72.00(14) y
N PD C3 C3A 100.81(14) y
C2 PD C3 C3A -110.5(2) y
CL PD C3 C3A -64.7(2) y
C7A PD C3 C3A -31.18(13) y
C2 C3 C3A C4 172.5(2) y
PD C3 C3A C4 -120.4(2) y
C2 C3 C3A C7A -12.0(3) y
PD C3 C3A C7A 55.15(18) y
C2 C3 C3A PD -67.14(15) y
C1 PD C3A C4 -152.0(3) y
N PD C3A C4 29.8(2) y
C2 PD C3A C4 162.7(3) y
C3 PD C3A C4 120.5(3) y
CL PD C3A C4 -85.2(2) y
C7A PD C3A C4 -115.4(3) y
C1 PD C3A C7A -36.64(14) y
N PD C3A C7A 145.16(13) y
C2 PD C3A C7A -81.91(16) y
C3 PD C3A C7A -124.2(2) y
CL PD C3A C7A 30.22(16) y
C1 PD C3A C3 87.53(16) y
N PD C3A C3 -90.67(14) y
C2 PD C3A C3 42.26(15) y
CL PD C3A C3 154.39(12) y
C7A PD C3A C3 124.2(2) y
C7A C3A C4 C5 -1.1(3) y
C3 C3A C4 C5 173.9(3) y
PD C3A C4 C5 91.5(3) y
C3A C4 C5 C6 -1.3(4) y
C4 C5 C6 C7 2.1(4) y
C5 C6 C7 C7A -0.2(4) y
C6 C7 C7A C3A -2.2(3) y
C6 C7 C7A C1 -176.1(2) y
C6 C7 C7A PD -98.3(3) y
C4 C3A C7A C7 3.0(3) y
C3 C3A C7A C7 -173.2(2) y
PD C3A C7A C7 -125.7(2) y
C4 C3A C7A C1 178.31(19) y
C3 C3A C7A C1 2.2(2) y
PD C3A C7A C1 49.62(14) y
C4 C3A C7A PD 128.7(2) y
C3 C3A C7A PD -47.44(15) y
C2 C1 C7A C7 -177.1(2) y
PD C1 C7A C7 113.1(3) y
C2 C1 C7A C3A 8.3(2) y
PD C1 C7A C3A -61.40(17) y
C2 C1 C7A PD 69.74(16) y
C1 PD C7A C7 -122.0(3) y
N PD C7A C7 69.8(2) y
C2 PD C7A C7 -164.2(2) y
C3 PD C7A C7 151.7(2) y
CL PD C7A C7 -39.7(2) y
C3A PD C7A C7 118.2(3) y
C1 PD C7A C3A 119.8(2) y
N PD C7A C3A -48.37(17) y
C2 PD C7A C3A 77.59(15) y
C3 PD C7A C3A 33.49(13) y
CL PD C7A C3A -157.90(12) y
N PD C7A C1 -168.21(14) y
C2 PD C7A C1 -42.25(15) y
C3 PD C7A C1 -86.36(16) y
CL PD C7A C1 82.26(14) y
C3A PD C7A C1 -119.8(2) y
C10 N C8 C9 65.3(2) y
C12 N C8 C9 -173.50(19) y
PD N C8 C9 -55.5(2) y
C8 N C10 C11 64.0(3) y
C12 N C10 C11 -55.2(3) y
PD N C10 C11 -174.36(16) y
C8 N C12 C13 177.41(19) y
C10 N C12 C13 -60.6(2) y
PD N C12 C13 58.6(2) y
