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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/15/7011594.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_7011594
loop_
_publ_author_name
'Liu, Ye'
'Lee, Kim Hun'
'Vittal, Jagadese J.'
'Hor, Tzi Sum Andy'
_publ_section_title
;
 Cleavage of homometallic and formation of heterometallic M--M bonds.
 Serendipitous syntheses of bimetallic
 MnPd(µ-PPh2)(CO)4(η2-P--P) (P--P = dppm, dppe, dppf) and
 polymetallic Mn2Pd2Ag(µ-Cl)(µ-PPh2)2(µ-dppm)(CO)8
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2747
_journal_paper_doi               10.1039/b202001g
_journal_year                    2002
_chemical_formula_sum            'C42 H34 Mn O4 P3 Pd'
_chemical_formula_weight         856.94
_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                92.3510(10)
_cell_angle_beta                 95.6200(10)
_cell_angle_gamma                94.8090(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0096(5)
_cell_length_b                   10.2022(5)
_cell_length_c                   18.7467(10)
_cell_measurement_reflns_used    6899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.34
_cell_volume                     1896.16(17)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD'
_diffrn_measurement_method       frames
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18173
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.8647
_exptl_absorpt_correction_T_min  0.7386
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin needle'
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         6660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0265
_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)+(0.0450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                5871
_reflns_number_total             6660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202001g.txt
_cod_data_source_block           pdmn
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011594
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.241771(16) 0.245169(16) 0.269759(9) 0.01493(7) Uani 1 1 d . . .
Mn1 Mn 0.48958(3) 0.35869(3) 0.265198(19) 0.01665(9) Uani 1 1 d . . .
P1 P 0.38544(6) 0.20261(6) 0.18609(3) 0.01507(13) Uani 1 1 d . . .
P2 P 0.15500(6) 0.33767(6) 0.36801(3) 0.01741(14) Uani 1 1 d . . .
P3 P 0.02957(6) 0.14404(6) 0.23802(3) 0.01705(14) Uani 1 1 d . . .
C1 C 0.5553(2) 0.2288(2) 0.31856(13) 0.0203(5) Uani 1 1 d . . .
O1 O 0.59717(17) 0.14862(17) 0.35435(9) 0.0270(4) Uani 1 1 d . . .
C2 C 0.3741(2) 0.4708(2) 0.22435(13) 0.0195(5) Uani 1 1 d . . .
O2 O 0.30198(17) 0.54288(17) 0.19926(10) 0.0273(4) Uani 1 1 d . . .
C3 C 0.6378(2) 0.4108(2) 0.22342(14) 0.0233(5) Uani 1 1 d . . .
O3 O 0.73128(19) 0.44576(18) 0.19558(11) 0.0368(5) Uani 1 1 d . . .
C4 C 0.5173(3) 0.4718(3) 0.34418(14) 0.0259(6) Uani 1 1 d . . .
O4 O 0.5370(2) 0.5441(2) 0.39321(11) 0.0412(5) Uani 1 1 d . . .
C5 C -0.0292(2) 0.3235(2) 0.34426(13) 0.0204(5) Uani 1 1 d . . .
H5A H -0.0750 0.3378 0.3880 0.024 Uiso 1 1 calc R . .
H5B H -0.0532 0.3922 0.3107 0.024 Uiso 1 1 calc R . .
C6 C -0.0776(2) 0.1870(2) 0.30916(13) 0.0219(5) Uani 1 1 d . . .
H6A H -0.1723 0.1868 0.2881 0.026 Uiso 1 1 calc R . .
H6B H -0.0740 0.1203 0.3460 0.026 Uiso 1 1 calc R . .
C1A C 0.4390(2) 0.0369(2) 0.17551(12) 0.0173(5) Uani 1 1 d . . .
C2A C 0.4372(2) -0.0466(2) 0.23246(13) 0.0217(5) Uani 1 1 d . . .
H2A H 0.4059 -0.0175 0.2761 0.026 Uiso 1 1 calc R . .
C3A C 0.4806(3) -0.1719(2) 0.22610(14) 0.0260(6) Uani 1 1 d . . .
H3A H 0.4801 -0.2278 0.2654 0.031 Uiso 1 1 calc R . .
C4A C 0.5246(3) -0.2153(2) 0.16188(14) 0.0282(6) Uani 1 1 d . . .
H4A H 0.5542 -0.3011 0.1573 0.034 Uiso 1 1 calc R . .
C5A C 0.5255(2) -0.1344(3) 0.10509(14) 0.0269(6) Uani 1 1 d . . .
H5A' H 0.5548 -0.1647 0.0611 0.032 Uiso 1 1 calc R . .
C6A C 0.4836(2) -0.0084(2) 0.11170(13) 0.0222(5) Uani 1 1 d . . .
H6A' H 0.4855 0.0473 0.0723 0.027 Uiso 1 1 calc R . .
C1B C 0.3301(2) 0.2427(2) 0.09447(12) 0.0180(5) Uani 1 1 d . . .
C2B C 0.3855(3) 0.3573(2) 0.06638(13) 0.0233(5) Uani 1 1 d . . .
H2B H 0.4582 0.4091 0.0932 0.028 Uiso 1 1 calc R . .
C3B C 0.3351(3) 0.3964(3) -0.00046(14) 0.0301(6) Uani 1 1 d . . .
H3B H 0.3729 0.4750 -0.0189 0.036 Uiso 1 1 calc R . .
C4B C 0.2308(3) 0.3214(3) -0.03982(14) 0.0317(6) Uani 1 1 d . . .
H4B H 0.1955 0.3490 -0.0851 0.038 Uiso 1 1 calc R . .
C5B C 0.1769(3) 0.2058(3) -0.01362(14) 0.0294(6) Uani 1 1 d . . .
H5B' H 0.1065 0.1529 -0.0415 0.035 Uiso 1 1 calc R . .
C6B C 0.2259(2) 0.1670(3) 0.05337(13) 0.0233(5) Uani 1 1 d . . .
H6B' H 0.1879 0.0880 0.0713 0.028 Uiso 1 1 calc R . .
C1C C 0.1850(2) 0.2444(2) 0.44787(12) 0.0203(5) Uani 1 1 d . . .
C2C C 0.3112(3) 0.1993(3) 0.46203(14) 0.0270(6) Uani 1 1 d . . .
H2C H 0.3767 0.2141 0.4292 0.032 Uiso 1 1 calc R . .
C3C C 0.3430(3) 0.1324(3) 0.52373(14) 0.0306(6) Uani 1 1 d . . .
H3C H 0.4303 0.1030 0.5332 0.037 Uiso 1 1 calc R . .
C4C C 0.2486(3) 0.1088(3) 0.57093(15) 0.0351(7) Uani 1 1 d . . .
H4C H 0.2703 0.0631 0.6131 0.042 Uiso 1 1 calc R . .
C5C C 0.1223(3) 0.1517(4) 0.55703(18) 0.0537(10) Uani 1 1 d . . .
H5C H 0.0565 0.1344 0.5895 0.064 Uiso 1 1 calc R . .
C6C C 0.0902(3) 0.2196(3) 0.49630(16) 0.0431(8) Uani 1 1 d . . .
H6C H 0.0030 0.2494 0.4876 0.052 Uiso 1 1 calc R . .
C1D C 0.1919(2) 0.5095(2) 0.39973(13) 0.0197(5) Uani 1 1 d . . .
C2D C 0.2452(3) 0.5475(3) 0.46946(14) 0.0293(6) Uani 1 1 d . . .
H2D H 0.2611 0.4828 0.5036 0.035 Uiso 1 1 calc R . .
C3D C 0.2751(3) 0.6802(3) 0.48911(15) 0.0361(7) Uani 1 1 d . . .
H3D H 0.3113 0.7058 0.5369 0.043 Uiso 1 1 calc R . .
C4D C 0.2529(3) 0.7753(3) 0.44019(16) 0.0335(7) Uani 1 1 d . . .
H4D H 0.2741 0.8659 0.4541 0.040 Uiso 1 1 calc R . .
C5D C 0.1996(3) 0.7382(3) 0.37070(15) 0.0307(6) Uani 1 1 d . . .
H5D H 0.1831 0.8033 0.3369 0.037 Uiso 1 1 calc R . .
C6D C 0.1705(3) 0.6060(2) 0.35042(13) 0.0251(6) Uani 1 1 d . . .
H6D H 0.1356 0.5809 0.3024 0.030 Uiso 1 1 calc R . .
C1E C -0.0031(2) -0.0344(2) 0.22448(12) 0.0181(5) Uani 1 1 d . . .
C2E C 0.0906(2) -0.1017(2) 0.19101(13) 0.0217(5) Uani 1 1 d . . .
H2E H 0.1670 -0.0542 0.1751 0.026 Uiso 1 1 calc R . .
C3E C 0.0735(3) -0.2379(2) 0.18062(14) 0.0251(6) Uani 1 1 d . . .
H3E H 0.1373 -0.2833 0.1571 0.030 Uiso 1 1 calc R . .
C4E C -0.0369(3) -0.3074(2) 0.20469(13) 0.0259(6) Uani 1 1 d . . .
H4E H -0.0482 -0.4007 0.1983 0.031 Uiso 1 1 calc R . .
C5E C -0.1305(3) -0.2416(2) 0.23785(14) 0.0265(6) Uani 1 1 d . . .
H5E H -0.2059 -0.2898 0.2544 0.032 Uiso 1 1 calc R . .
C6E C -0.1150(2) -0.1051(2) 0.24723(13) 0.0237(5) Uani 1 1 d . . .
H6E H -0.1808 -0.0600 0.2692 0.028 Uiso 1 1 calc R . .
C1F C -0.0507(2) 0.2082(2) 0.15666(12) 0.0187(5) Uani 1 1 d . . .
C2F C -0.0002(2) 0.3304(2) 0.13530(13) 0.0206(5) Uani 1 1 d . . .
H2F H 0.0734 0.3782 0.1635 0.025 Uiso 1 1 calc R . .
C3F C -0.0559(3) 0.3828(3) 0.07366(14) 0.0261(6) Uani 1 1 d . . .
H3F H -0.0219 0.4670 0.0603 0.031 Uiso 1 1 calc R . .
C4F C -0.1615(3) 0.3122(3) 0.03124(14) 0.0298(6) Uani 1 1 d . . .
H4F H -0.1990 0.3475 -0.0116 0.036 Uiso 1 1 calc R . .
C5F C -0.2121(3) 0.1904(3) 0.05153(15) 0.0332(7) Uani 1 1 d . . .
H5F H -0.2841 0.1421 0.0224 0.040 Uiso 1 1 calc R . .
C6F C -0.1578(3) 0.1385(3) 0.11431(14) 0.0278(6) Uani 1 1 d . . .
H6F H -0.1938 0.0554 0.1283 0.033 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 0.0033 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'
Mn Mn 0.3368 0.7283 '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'
P P 0.1023 0.0942 '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'
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
P1 Pd1 P3 111.81(2) . . ?
P1 Pd1 P2 161.13(2) . . ?
P3 Pd1 P2 86.74(2) . . ?
P1 Pd1 Mn1 53.428(17) . . ?
P3 Pd1 Mn1 163.204(19) . . ?
P2 Pd1 Mn1 107.706(18) . . ?
C3 Mn1 C1 99.44(11) . . ?
C3 Mn1 C4 98.40(11) . . ?
C1 Mn1 C4 89.78(11) . . ?
C3 Mn1 C2 99.14(11) . . ?
C1 Mn1 C2 161.41(11) . . ?
C4 Mn1 C2 88.18(11) . . ?
C3 Mn1 P1 102.46(8) . . ?
C1 Mn1 P1 88.67(7) . . ?
C4 Mn1 P1 159.06(9) . . ?
C2 Mn1 P1 86.68(7) . . ?
C3 Mn1 Pd1 155.61(8) . . ?
C1 Mn1 Pd1 89.21(7) . . ?
C4 Mn1 Pd1 104.43(8) . . ?
C2 Mn1 Pd1 73.45(7) . . ?
P1 Mn1 Pd1 54.667(17) . . ?
C1A P1 C1B 103.54(11) . . ?
C1A P1 Mn1 124.01(8) . . ?
C1B P1 Mn1 120.67(8) . . ?
C1A P1 Pd1 119.29(8) . . ?
C1B P1 Pd1 115.66(7) . . ?
Mn1 P1 Pd1 71.91(2) . . ?
C1C P2 C1D 104.61(11) . . ?
C1C P2 C5 106.46(11) . . ?
C1D P2 C5 103.13(11) . . ?
C1C P2 Pd1 112.23(8) . . ?
C1D P2 Pd1 123.95(8) . . ?
C5 P2 Pd1 104.98(8) . . ?
C1E P3 C1F 104.28(10) . . ?
C1E P3 C6 103.98(11) . . ?
C1F P3 C6 104.74(11) . . ?
C1E P3 Pd1 122.40(8) . . ?
C1F P3 Pd1 112.08(8) . . ?
C6 P3 Pd1 107.82(8) . . ?
O1 C1 Mn1 178.0(2) . . ?
O2 C2 Mn1 179.1(2) . . ?
O3 C3 Mn1 178.5(2) . . ?
O4 C4 Mn1 178.6(3) . . ?
C6 C5 P2 110.59(16) . . ?
C5 C6 P3 110.44(16) . . ?
C6A C1A C2A 118.7(2) . . ?
C6A C1A P1 121.49(18) . . ?
C2A C1A P1 119.84(18) . . ?
C3A C2A C1A 120.8(2) . . ?
C2A C3A C4A 119.7(2) . . ?
C5A C4A C3A 120.1(2) . . ?
C4A C5A C6A 120.3(2) . . ?
C5A C6A C1A 120.5(2) . . ?
C6B C1B C2B 118.5(2) . . ?
C6B C1B P1 121.46(19) . . ?
C2B C1B P1 119.79(18) . . ?
C3B C2B C1B 120.6(2) . . ?
C4B C3B C2B 120.0(3) . . ?
C3B C4B C5B 120.2(2) . . ?
C4B C5B C6B 120.0(2) . . ?
C5B C6B C1B 120.6(2) . . ?
C2C C1C C6C 118.4(2) . . ?
C2C C1C P2 117.74(19) . . ?
C6C C1C P2 123.80(19) . . ?
C1C C2C C3C 120.8(2) . . ?
C4C C3C C2C 120.1(2) . . ?
C3C C4C C5C 119.7(3) . . ?
C4C C5C C6C 120.6(3) . . ?
C5C C6C C1C 120.3(3) . . ?
C2D C1D C6D 119.1(2) . . ?
C2D C1D P2 123.03(19) . . ?
C6D C1D P2 117.82(18) . . ?
C3D C2D C1D 119.8(2) . . ?
C4D C3D C2D 120.8(3) . . ?
C3D C4D C5D 119.6(2) . . ?
C4D C5D C6D 120.0(3) . . ?
C5D C6D C1D 120.6(2) . . ?
C2E C1E C6E 119.2(2) . . ?
C2E C1E P3 117.64(18) . . ?
C6E C1E P3 123.17(19) . . ?
C3E C2E C1E 120.6(2) . . ?
C4E C3E C2E 119.7(2) . . ?
C5E C4E C3E 120.2(2) . . ?
C4E C5E C6E 120.3(2) . . ?
C5E C6E C1E 120.1(2) . . ?
C6F C1F C2F 119.0(2) . . ?
C6F C1F P3 122.64(19) . . ?
C2F C1F P3 118.36(18) . . ?
C3F C2F C1F 120.8(2) . . ?
C2F C3F C4F 120.0(2) . . ?
C5F C4F C3F 119.8(2) . . ?
C4F C5F C6F 120.3(2) . . ?
C5F C6F C1F 120.1(2) . . ?
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
Pd1 P1 2.2820(6) . ?
Pd1 P3 2.2945(6) . ?
Pd1 P2 2.3121(6) . ?
Pd1 Mn1 2.6589(4) . ?
Mn1 C3 1.796(3) . ?
Mn1 C1 1.820(3) . ?
Mn1 C4 1.824(3) . ?
Mn1 C2 1.831(3) . ?
Mn1 P1 2.2465(7) . ?
P1 C1A 1.825(2) . ?
P1 C1B 1.826(2) . ?
P2 C1C 1.820(2) . ?
P2 C1D 1.824(2) . ?
P2 C5 1.846(2) . ?
P3 C1E 1.825(2) . ?
P3 C1F 1.825(2) . ?
P3 C6 1.853(2) . ?
C1 O1 1.159(3) . ?
C2 O2 1.154(3) . ?
C3 O3 1.153(3) . ?
C4 O4 1.145(3) . ?
C5 C6 1.535(3) . ?
C1A C6A 1.392(3) . ?
C1A C2A 1.394(3) . ?
C2A C3A 1.389(3) . ?
C3A C4A 1.390(4) . ?
C4A C5A 1.374(4) . ?
C5A C6A 1.390(3) . ?
C1B C6B 1.392(3) . ?
C1B C2B 1.397(3) . ?
C2B C3B 1.391(3) . ?
C3B C4B 1.375(4) . ?
C4B C5B 1.384(4) . ?
C5B C6B 1.388(4) . ?
C1C C2C 1.385(3) . ?
C1C C6C 1.392(4) . ?
C2C C3C 1.390(4) . ?
C3C C4C 1.370(4) . ?
C4C C5C 1.377(4) . ?
C5C C6C 1.381(4) . ?
C1D C2D 1.389(3) . ?
C1D C6D 1.393(3) . ?
C2D C3D 1.389(4) . ?
C3D C4D 1.379(4) . ?
C4D C5D 1.384(4) . ?
C5D C6D 1.385(4) . ?
C1E C2E 1.391(3) . ?
C1E C6E 1.393(3) . ?
C2E C3E 1.389(3) . ?
C3E C4E 1.386(4) . ?
C4E C5E 1.378(4) . ?
C5E C6E 1.391(4) . ?
C1F C6F 1.394(3) . ?
C1F C2F 1.395(3) . ?
C2F C3F 1.380(3) . ?
C3F C4F 1.389(4) . ?
C4F C5F 1.384(4) . ?
C5F C6F 1.391(4) . ?
