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#$Date: 2016-03-22 12:48:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178964 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/93/4119306.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_4119306
loop_
_publ_author_name
'Christophe Werlé'
'Mustapha Hamdaoui'
'Corinne Bailly'
'Xavier-Frédéric Le Goff'
'Lydia Brelot'
'Jean-Pierre Djukic'
_publ_contact_author_address
;Institut de Chimie
Universite de Strasbourg
4 rue Blaise Pascal
67000 Strasbourg 
France
;
_publ_contact_author_email       djukic@unistra.fr
_publ_contact_author_name        'J.P. Djukic'
_publ_contact_author_phone       33(0)368851523
_publ_section_title
;
 Electron-Deficient η1-Indenyl,η3-allylpalladium(II) Complexes
 Stabilized by Fluxional Non-covalent Interactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1715
_journal_page_last               1718
_journal_paper_doi               10.1021/ja312003q
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C26 H18 Cr2 O6'
_chemical_formula_sum            'C26 H18 Cr2 O6'
_chemical_formula_weight         530.40
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.936(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.165(1)
_cell_length_b                   7.513(1)
_cell_length_c                   13.761(1)
_cell_measurement_reflns_used    624
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2324.5(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7378
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.9620
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0367
_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)+(0.0338P)²+3.9518P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                3045
_reflns_number_total             3366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312003q_si_002_11.cif
_cod_data_source_block           5d
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4119306
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Cr1 Cr 0.141249(11) 0.95427(3) 0.176126(19) 0.01896(9) Uani 1 1 d .
O1 O 0.17850(7) 0.5750(2) 0.16780(14) 0.0425(4) Uani 1 1 d .
O2 O 0.23888(6) 1.0594(2) 0.07964(12) 0.0439(4) Uani 1 1 d .
O3 O 0.05979(7) 0.8897(2) -0.02500(11) 0.0387(3) Uani 1 1 d .
C1 C 0.12992(7) 0.9021(2) 0.33176(12) 0.0226(3) Uani 1 1 d .
C2 C 0.17918(8) 1.0154(3) 0.33877(13) 0.0276(4) Uani 1 1 d .
H2 H 0.2170 0.9855 0.3801 0.033 Uiso 1 1 d R
C3 C 0.17074(8) 1.1744(3) 0.28275(15) 0.0293(4) Uani 1 1 d .
H3 H 0.2034 1.2527 0.2867 0.035 Uiso 1 1 d R
C4 C 0.11475(8) 1.2195(2) 0.22098(15) 0.0274(4) Uani 1 1 d .
H4 H 0.1098 1.3290 0.1855 0.033 Uiso 1 1 d R
C5 C 0.06608(7) 1.1024(2) 0.21172(13) 0.0225(3) Uani 1 1 d .
H5 H 0.0289 1.1288 0.1671 0.027 Uiso 1 1 d R
C6 C 0.07347(7) 0.9462(2) 0.26960(12) 0.0194(3) Uani 1 1 d .
C7 C 0.03135(7) 0.8040(2) 0.27795(12) 0.0200(3) Uani 1 1 d .
C8 C 0.05946(7) 0.6822(2) 0.34458(13) 0.0228(3) Uani 1 1 d .
C9 C 0.12408(7) 0.7308(3) 0.38460(13) 0.0266(3) Uani 1 1 d .
H9A H 0.1336 0.7478 0.4581 0.032 Uiso 1 1 calc R
H9B H 0.1505 0.6379 0.3682 0.032 Uiso 1 1 calc R
C10 C 0.03360(9) 0.5195(3) 0.37947(16) 0.0330(4) Uani 1 1 d .
H10A H -0.0098 0.5222 0.3554 0.050 Uiso 1 1 calc R
H10B H 0.0443 0.5158 0.4528 0.050 Uiso 1 1 calc R
H10C H 0.0493 0.4136 0.3531 0.050 Uiso 1 1 calc R
C12 C 0.16455(8) 0.7222(2) 0.17188(14) 0.0271(4) Uani 1 1 d .
C13 C 0.20113(8) 1.0190(3) 0.11678(14) 0.0277(4) Uani 1 1 d .
C14 C 0.09139(7) 0.9162(2) 0.05214(14) 0.0252(3) Uani 1 1 d .
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'
Cr Cr 0.3209 0.6236 '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'
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_3
C12 Cr1 C13 88.74(9) .
C12 Cr1 C14 86.93(8) .
C13 Cr1 C14 90.08(8) .
C12 Cr1 C3 133.51(8) .
C13 Cr1 C3 87.20(8) .
C14 Cr1 C3 139.32(8) .
C12 Cr1 C4 165.71(8) .
C13 Cr1 C4 100.10(8) .
C14 Cr1 C4 104.13(8) .
C3 Cr1 C4 37.18(7) .
C12 Cr1 C5 137.57(7) .
C13 Cr1 C5 133.03(8) .
C14 Cr1 C5 86.09(7) .
C3 Cr1 C5 67.12(7) .
C4 Cr1 C5 37.12(6) .
C12 Cr1 C2 100.30(8) .
C13 Cr1 C2 103.46(7) .
C14 Cr1 C2 164.68(7) .
C3 Cr1 C2 36.90(7) .
C4 Cr1 C2 66.85(7) .
C5 Cr1 C2 79.45(7) .
C12 Cr1 C1 88.13(8) .
C13 Cr1 C1 137.88(7) .
C14 Cr1 C1 131.62(7) .
C3 Cr1 C1 65.60(7) .
C4 Cr1 C1 77.78(7) .
C5 Cr1 C1 66.44(6) .
C2 Cr1 C1 36.47(6) .
C12 Cr1 C6 104.08(7) .
C13 Cr1 C6 164.56(8) .
C14 Cr1 C6 99.03(7) .
C3 Cr1 C6 77.75(6) .
C4 Cr1 C6 65.69(6) .
C5 Cr1 C6 36.60(6) .
C2 Cr1 C6 66.21(6) .
C1 Cr1 C6 36.66(6) .
C2 C1 C6 120.96(16) .
C2 C1 C9 130.66(15) .
C6 C1 C9 108.35(14) .
C2 C1 Cr1 71.46(10) .
C6 C1 Cr1 71.81(9) .
C9 C1 Cr1 130.88(13) .
C1 C2 C3 118.13(16) .
C1 C2 Cr1 72.07(10) .
C3 C2 Cr1 70.05(10) .
C1 C2 H2 120.9 .
C3 C2 H2 120.9 .
Cr1 C2 H2 129.1 .
C2 C3 C4 121.30(16) .
C2 C3 Cr1 73.05(11) .
C4 C3 Cr1 71.75(10) .
C2 C3 H3 119.4 .
C4 C3 H3 119.3 .
Cr1 C3 H3 128.1 .
C3 C4 C5 120.24(17) .
C3 C4 Cr1 71.07(11) .
C5 C4 Cr1 71.54(10) .
C3 C4 H4 119.9 .
C5 C4 H4 119.9 .
Cr1 C4 H4 130.0 .
C6 C5 C4 118.92(16) .
C6 C5 Cr1 73.21(9) .
C4 C5 Cr1 71.34(10) .
C6 C5 H5 120.5 .
C4 C5 H5 120.5 .
Cr1 C5 H5 126.8 .
C5 C6 C1 120.35(15) .
C5 C6 C7 131.19(15) .
C1 C6 C7 108.44(14) .
C5 C6 Cr1 70.19(9) .
C1 C6 Cr1 71.53(9) .
C7 C6 Cr1 129.06(11) .
C8 C7 C6 109.01(14) .
C8 C7 C7 127.62(13) 2
C6 C7 C7 123.36(12) 2
C7 C8 C10 127.63(16) .
C7 C8 C9 110.99(15) .
C10 C8 C9 121.37(16) .
C1 C9 C8 103.16(13) .
C1 C9 H9A 111.1 .
C8 C9 H9A 111.1 .
C1 C9 H9B 111.1 .
C8 C9 H9B 111.1 .
H9A C9 H9B 109.1 .
C8 C10 H10A 109.5 .
C8 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
C8 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
O1 C12 Cr1 178.8(2) .
O2 C13 Cr1 179.8(2) .
O3 C14 Cr1 178.81(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 C12 1.8306(19) .
Cr1 C13 1.8367(18) .
Cr1 C14 1.8379(18) .
Cr1 C3 2.2071(18) .
Cr1 C4 2.2159(19) .
Cr1 C5 2.2185(16) .
Cr1 C2 2.2461(18) .
Cr1 C1 2.2539(17) .
Cr1 C6 2.2576(16) .
O1 C12 1.157(2) .
O2 C13 1.155(2) .
O3 C14 1.152(2) .
C1 C2 1.408(2) .
C1 C6 1.419(2) .
C1 C9 1.500(3) .
C2 C3 1.410(3) .
C2 H2 0.9499 .
C3 C4 1.410(3) .
C3 H3 0.9499 .
C4 C5 1.411(2) .
C4 H4 0.9500 .
C5 C6 1.406(2) .
C5 H5 0.9501 .
C6 C7 1.469(2) .
C7 C8 1.347(2) .
C7 C7 1.471(3) 2
C8 C10 1.491(3) .
C8 C9 1.510(2) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
