#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:49:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179426 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/23/4332393.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332393
loop_
_publ_author_name
'Croizat, Pierre'
'Auvray, Nicolas'
'Braunstein, Pierre'
'Welter, Richard'
_publ_section_title
;
 Comparative Bonding Behavior of Functional Cyclopentadienyl Ligands and
 Boron-Containing Analogues in Heterometallic Complexes and
 Clusters†
;
_journal_issue                   15
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5852
_journal_page_last               5866
_journal_paper_doi               10.1021/ic060318d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C32 H50 Mo2 N2 O6 P2 Pd2'
_chemical_formula_sum            'C32 H50 Mo2 N2 O6 P2 Pd2'
_chemical_formula_weight         1025.36
_chemical_name_systematic
; 
 ? 
;
_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                106.08(5)
_cell_angle_beta                 99.15(5)
_cell_angle_gamma                102.49(5)
_cell_formula_units_Z            1
_cell_length_a                   9.2080(10)
_cell_length_b                   9.9380(10)
_cell_length_c                   11.0610(10)
_cell_measurement_reflns_used    5223
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     923.3(5)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6560
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.053
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0355
_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/[σ²(Fo²)+(0.0503P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                4039
_reflns_number_total             5185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060318dsup5.cif
_cod_data_source_block           shelxs97
_cod_original_cell_volume        923.35(46)
_cod_database_code               4332393
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pd Pd 0.41953(3) 0.89128(3) 0.89964(2) 0.01865(8) Uani 1 1 d
Mo Mo 0.41440(3) 0.85173(3) 1.14075(3) 0.01913(9) Uani 1 1 d
P P 0.27598(10) 0.68069(10) 0.73448(9) 0.02313(19) Uani 1 1 d
O1 O 0.7199(3) 1.0231(3) 1.3389(3) 0.0355(6) Uani 1 1 d
O2 O 0.5999(3) 0.6853(3) 0.9708(3) 0.0318(6) Uani 1 1 d
O3 O 0.2158(3) 1.0450(3) 1.0528(3) 0.0342(6) Uani 1 1 d
N N 0.0828(3) 0.8640(4) 1.2571(3) 0.0316(7) Uani 1 1 d
C1 C 0.6115(4) 0.9817(4) 1.2533(4) 0.0230(7) Uani 1 1 d
C2 C 0.5281(4) 0.7570(4) 1.0212(3) 0.0231(7) Uani 1 1 d
C3 C 0.3074(4) 0.9836(4) 1.0722(4) 0.0255(7) Uani 1 1 d
C4 C 0.1941(4) 0.6759(4) 1.1340(4) 0.0316(8) Uani 1 1 d
H4 H 0.1170 0.6341 1.0558 0.038 Uiso 1 1 calc
C5 C 0.3251(5) 0.6278(4) 1.1642(5) 0.0405(10) Uani 1 1 d
H5 H 0.3479 0.5449 1.1125 0.049 Uiso 1 1 calc
C6 C 0.4149(4) 0.7239(5) 1.2832(4) 0.0359(10) Uani 1 1 d
H6 H 0.5098 0.7177 1.3265 0.043 Uiso 1 1 calc
C7 C 0.3406(4) 0.8332(4) 1.3292(4) 0.0282(8) Uani 1 1 d
H7 H 0.3801 0.9152 1.4055 0.034 Uiso 1 1 calc
C8 C 0.1969(4) 0.7980(4) 1.2410(4) 0.0253(7) Uani 1 1 d
C9 C 0.1174(5) 1.0049(5) 1.3547(5) 0.0417(10) Uani 1 1 d
H9A H 0.0248 1.0384 1.3541 0.062 Uiso 1 1 calc
H9B H 0.1965 1.0747 1.3362 0.062 Uiso 1 1 calc
H9C H 0.1544 0.9972 1.4399 0.062 Uiso 1 1 calc
C10 C -0.0430(4) 0.8306(5) 1.1446(5) 0.0419(11) Uani 1 1 d
H10A H -0.1160 0.8857 1.1692 0.063 Uiso 1 1 calc
H10B H -0.0948 0.7261 1.1140 0.063 Uiso 1 1 calc
H10C H -0.0022 0.8577 1.0755 0.063 Uiso 1 1 calc
C11 C 0.0751(4) 0.6704(4) 0.6742(4) 0.0333(9) Uani 1 1 d
H11A H 0.0708 0.7510 0.6388 0.040 Uiso 1 1 calc
H11B H 0.0271 0.5776 0.6027 0.040 Uiso 1 1 calc
C12 C -0.0158(4) 0.6792(6) 0.7772(5) 0.0519(13) Uani 1 1 d
H12A H -0.1224 0.6702 0.7388 0.078 Uiso 1 1 calc
H12B H 0.0277 0.7731 0.8462 0.078 Uiso 1 1 calc
H12C H -0.0116 0.6001 0.8132 0.078 Uiso 1 1 calc
C13 C 0.3505(5) 0.6553(4) 0.5882(4) 0.0325(8) Uani 1 1 d
H13A H 0.2944 0.5586 0.5248 0.039 Uiso 1 1 calc
H13B H 0.3334 0.7303 0.5488 0.039 Uiso 1 1 calc
C14 C 0.5212(5) 0.6664(5) 0.6187(5) 0.0482(12) Uani 1 1 d
H14A H 0.5582 0.6544 0.5391 0.072 Uiso 1 1 calc
H14B H 0.5379 0.5899 0.6548 0.072 Uiso 1 1 calc
H14C H 0.5769 0.7620 0.6817 0.072 Uiso 1 1 calc
C15 C 0.2677(4) 0.5080(4) 0.7673(4) 0.0310(8) Uani 1 1 d
H15A H 0.3739 0.5036 0.7944 0.037 Uiso 1 1 calc
H15B H 0.2199 0.5096 0.8415 0.037 Uiso 1 1 calc
C16 C 0.1814(5) 0.3684(4) 0.6563(4) 0.0383(10) Uani 1 1 d
H16A H 0.1849 0.2839 0.6849 0.057 Uiso 1 1 calc
H16B H 0.2292 0.3629 0.5827 0.057 Uiso 1 1 calc
H16C H 0.0747 0.3687 0.6302 0.057 Uiso 1 1 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mo Mo -1.6832 0.6857 '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'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 '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
P Pd C3 117.93(10) . .
P Pd C1 87.13(10) . 2_677
C3 Pd C1 109.22(12) . 2_677
P Pd C2 92.44(9) . .
C3 Pd C2 89.05(12) . .
C1 Pd C2 159.52(12) 2_677 .
P Pd C3 126.18(11) . 2_677
C3 Pd C3 115.49(10) . 2_677
C1 Pd C3 81.48(12) 2_677 2_677
C2 Pd C3 82.30(12) . 2_677
P Pd Pd 173.69(3) . 2_677
C3 Pd Pd 59.81(9) . 2_677
C1 Pd Pd 99.17(9) 2_677 2_677
C2 Pd Pd 81.75(9) . 2_677
C3 Pd Pd 55.69(10) 2_677 2_677
P Pd Mo 109.99(5) . .
C3 Pd Mo 45.28(8) . .
C1 Pd Mo 153.58(9) 2_677 .
C2 Pd Mo 43.79(9) . .
C3 Pd Mo 102.42(10) 2_677 .
Pd Pd Mo 64.03(4) 2_677 .
P Pd Mo 124.26(4) . 2_677
C3 Pd Mo 103.58(9) . 2_677
C1 Pd Mo 42.86(9) 2_677 2_677
C2 Pd Mo 125.27(8) . 2_677
C3 Pd Mo 43.96(9) 2_677 2_677
Pd Pd Mo 61.68(4) 2_677 2_677
Mo Pd Mo 125.71(5) . 2_677
C1 Mo C2 88.73(15) . .
C1 Mo C3 105.10(15) . .
C2 Mo C3 112.81(15) . .
C1 Mo C6 86.88(15) . .
C2 Mo C6 101.63(15) . .
C3 Mo C6 143.48(15) . .
C1 Mo C5 118.70(16) . .
C2 Mo C5 86.65(15) . .
C3 Mo C5 132.58(15) . .
C6 Mo C5 35.44(17) . .
C1 Mo C7 87.06(14) . .
C2 Mo C7 137.52(14) . .
C3 Mo C7 109.08(14) . .
C6 Mo C7 35.94(14) . .
C5 Mo C7 59.22(16) . .
C1 Mo C4 143.55(14) . .
C2 Mo C4 108.46(15) . .
C3 Mo C4 97.57(14) . .
C6 Mo C4 58.74(15) . .
C5 Mo C4 35.44(14) . .
C7 Mo C4 58.36(14) . .
C1 Mo C8 118.33(14) . .
C2 Mo C8 142.24(14) . .
C3 Mo C8 86.54(13) . .
C6 Mo C8 57.94(13) . .
C5 Mo C8 57.97(14) . .
C7 Mo C8 34.33(12) . .
C4 Mo C8 34.49(13) . .
C1 Mo Pd 103.74(11) . .
C2 Mo Pd 56.93(10) . .
C3 Mo Pd 55.90(11) . .
C6 Mo Pd 155.08(12) . .
C5 Mo Pd 123.19(14) . .
C7 Mo Pd 163.10(9) . .
C4 Mo Pd 112.61(11) . .
C8 Mo Pd 130.02(9) . .
C1 Mo Pd 55.60(11) . 2_677
C2 Mo Pd 82.56(10) . 2_677
C3 Mo Pd 57.84(10) . 2_677
C6 Mo Pd 142.32(12) . 2_677
C5 Mo Pd 167.80(10) . 2_677
C7 Mo Pd 127.32(11) . 2_677
C4 Mo Pd 155.35(10) . 2_677
C8 Mo Pd 133.81(9) . 2_677
Pd Mo Pd 54.29(5) . 2_677
C13 P C11 102.9(2) . .
C13 P C15 103.02(19) . .
C11 P C15 104.10(19) . .
C13 P Pd 112.24(14) . .
C11 P Pd 116.45(14) . .
C15 P Pd 116.46(13) . .
C8 N C9 119.0(3) . .
C8 N C10 117.8(4) . .
C9 N C10 117.0(3) . .
O1 C1 Mo 157.4(3) . .
O1 C1 Pd 121.0(3) . 2_677
Mo C1 Pd 81.54(13) . 2_677
O2 C2 Mo 164.8(3) . .
O2 C2 Pd 115.8(3) . .
Mo C2 Pd 79.28(12) . .
O3 C3 Mo 159.9(3) . .
O3 C3 Pd 117.5(3) . .
Mo C3 Pd 78.83(13) . .
O3 C3 Pd 118.5(3) . 2_677
Mo C3 Pd 78.20(11) . 2_677
Pd C3 Pd 64.51(10) . 2_677
C5 C4 C8 108.7(4) . .
C5 C4 Mo 70.4(2) . .
C8 C4 Mo 77.3(2) . .
C5 C4 H4 125.6 . .
C8 C4 H4 125.6 . .
Mo C4 H4 118.5 . .
C6 C5 C4 107.9(4) . .
C6 C5 Mo 71.6(2) . .
C4 C5 Mo 74.2(2) . .
C6 C5 H5 126.1 . .
C4 C5 H5 126.1 . .
Mo C5 H5 120.0 . .
C5 C6 C7 108.6(3) . .
C5 C6 Mo 73.0(2) . .
C7 C6 Mo 74.0(2) . .
C5 C6 H6 125.7 . .
C7 C6 H6 125.7 . .
Mo C6 H6 119.1 . .
C8 C7 C6 108.2(4) . .
C8 C7 Mo 78.0(2) . .
C6 C7 Mo 70.0(2) . .
C8 C7 H7 125.9 . .
C6 C7 H7 125.9 . .
Mo C7 H7 117.9 . .
N C8 C7 126.9(4) . .
N C8 C4 126.9(3) . .
C7 C8 C4 106.2(3) . .
N C8 Mo 130.4(2) . .
C7 C8 Mo 67.65(19) . .
C4 C8 Mo 68.2(2) . .
N C9 H9A 109.5 . .
N C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N C10 H10A 109.5 . .
N C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 P 113.2(3) . .
C12 C11 H11A 108.9 . .
P C11 H11A 108.9 . .
C12 C11 H11B 108.9 . .
P C11 H11B 108.9 . .
H11A C11 H11B 107.7 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C14 C13 P 111.3(3) . .
C14 C13 H13A 109.4 . .
P C13 H13A 109.4 . .
C14 C13 H13B 109.4 . .
P C13 H13B 109.4 . .
H13A C13 H13B 108.0 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C16 C15 P 116.8(3) . .
C16 C15 H15A 108.1 . .
P C15 H15A 108.1 . .
C16 C15 H15B 108.1 . .
P C15 H15B 108.1 . .
H15A C15 H15B 107.3 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd P 2.320(2) .
Pd C3 2.370(4) .
Pd C1 2.392(3) 2_677
Pd C2 2.395(4) .
Pd C3 2.480(4) 2_677
Pd Pd 2.590(2) 2_677
Pd Mo 2.8075(5) .
Pd Mo 2.8672(13) 2_677
Mo C1 1.972(4) .
Mo C2 1.977(4) .
Mo C3 2.033(3) .
Mo C6 2.282(4) .
Mo C5 2.300(4) .
Mo C7 2.334(4) .
Mo C4 2.350(4) .
Mo C8 2.469(3) .
Mo Pd 2.8672(13) 2_677
P C13 1.831(4) .
P C11 1.834(4) .
P C15 1.838(4) .
O1 C1 1.170(4) .
O2 C2 1.165(4) .
O3 C3 1.169(4) .
N C8 1.364(5) .
N C9 1.445(6) .
N C10 1.465(5) .
C1 Pd 2.392(3) 2_677
C3 Pd 2.480(4) 2_677
C4 C5 1.416(6) .
C4 C8 1.433(6) .
C4 H4 0.9500 .
C5 C6 1.395(7) .
C5 H5 0.9500 .
C6 C7 1.425(6) .
C6 H6 0.9500 .
C7 C8 1.423(5) .
C7 H7 0.9500 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.511(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.527(6) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.527(6) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
