#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:07:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179776 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007236.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_7007236
loop_
_publ_author_name
'Auvray, Nicolas'
'Basu Baul, Tushar S.'
'Braunstein, Pierre'
'Croizat, Pierre'
'Englert, Ulli'
'Herberich, Gerhard E.'
'Welter, Richard'
_publ_section_title
;
 Organometallic building blocks with amino-substituted cyclopentadienyl
 and boratabenzene ligands for the synthesis of heterometallic
 complexes and clusters.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2950
_journal_page_last               2958
_journal_paper_doi               10.1039/b602106a
_journal_year                    2006
_chemical_formula_moiety         'C34 H30 Mo2 N4 O6 Pt, 2(O C4 H8)'
_chemical_formula_sum            'C42 H46 Mo2 N4 O8 Pt'
_chemical_formula_weight         1121.80
_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                94.91(5)
_cell_angle_beta                 109.36(5)
_cell_angle_gamma                107.20(5)
_cell_formula_units_Z            1
_cell_length_a                   8.518(5)
_cell_length_b                   11.117(5)
_cell_length_c                   12.785(5)
_cell_measurement_reflns_used    22809
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      1.018
_cell_volume                     1068.2(11)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1680
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6095
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    3.899
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.060
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0744
_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)+(0.0367P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                3564
_reflns_number_total             6094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602106a.txt
_cod_data_source_block           croizat
_cod_original_cell_volume        1068.3(9)
_cod_database_code               7007236
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
Pt Pt 0.0000 0.0000 0.5000 0.04091(19) Uani 1 2 d S . .
Mo Mo -0.32287(10) -0.09476(6) 0.30588(6) 0.0420(2) Uani 1 1 d . . .
O1 O -0.3692(10) -0.1021(7) 0.5390(6) 0.0632(19) Uani 1 1 d . . .
O2 O 0.0084(10) -0.1385(7) 0.2792(6) 0.0596(18) Uani 1 1 d . . .
O3 O -0.4465(13) -0.3926(7) 0.2675(7) 0.088(3) Uani 1 1 d . . .
O4 O 0.0774(15) 0.2528(9) 0.1892(9) 0.106(3) Uani 1 1 d . . .
N1 N 0.0236(11) 0.1697(7) 0.4655(6) 0.0478(19) Uani 1 1 d . . .
N2 N -0.6995(13) -0.2065(9) 0.0658(8) 0.063(2) Uani 1 1 d . . .
C1 C -0.3392(13) -0.0988(9) 0.4567(9) 0.050(2) Uani 1 1 d . . .
C2 C -0.1047(14) -0.1161(8) 0.2990(8) 0.046(2) Uani 1 1 d . . .
C3 C -0.3980(15) -0.2796(10) 0.2851(9) 0.060(3) Uani 1 1 d . . .
C4 C -0.5724(14) -0.0339(10) 0.2344(9) 0.058(3) Uani 1 1 d . . .
H4 H -0.6623 -0.0597 0.2646 0.070 Uiso 1 1 calc . . .
C5 C -0.4164(15) 0.0796(10) 0.2804(9) 0.055(2) Uani 1 1 d . . .
H5 H -0.3874 0.1445 0.3439 0.066 Uiso 1 1 calc . . .
C6 C -0.3161(13) 0.0765(9) 0.2146(9) 0.053(2) Uani 1 1 d . . .
H6 H -0.2058 0.1399 0.2256 0.064 Uiso 1 1 calc . . .
C7 C -0.4042(13) -0.0358(9) 0.1286(7) 0.048(2) Uani 1 1 d . . .
H7 H -0.3609 -0.0635 0.0748 0.057 Uiso 1 1 calc . . .
C8 C -0.5687(14) -0.0999(9) 0.1371(8) 0.051(2) Uani 1 1 d . . .
C9 C -0.8306(16) -0.2863(12) 0.1045(10) 0.077(3) Uani 1 1 d . . .
H9A H -0.7930 -0.3566 0.1324 0.115 Uiso 1 1 calc . . .
H9B H -0.9457 -0.3220 0.0413 0.115 Uiso 1 1 calc . . .
H9C H -0.8411 -0.2337 0.1657 0.115 Uiso 1 1 calc . . .
C10 C -0.6500(16) -0.2843(10) -0.0080(8) 0.066(3) Uani 1 1 d . . .
H10A H -0.6287 -0.2387 -0.0670 0.099 Uiso 1 1 calc . . .
H10B H -0.7463 -0.3671 -0.0433 0.099 Uiso 1 1 calc . . .
H10C H -0.5419 -0.2991 0.0371 0.099 Uiso 1 1 calc . . .
C11 C 0.0514(13) 0.2723(8) 0.4484(8) 0.046(2) Uani 1 1 d . . .
C12 C 0.0953(14) 0.4025(8) 0.4289(8) 0.050(2) Uani 1 1 d . . .
C13 C -0.0250(14) 0.4404(9) 0.3499(9) 0.057(2) Uani 1 1 d . . .
H13 H -0.1398 0.3807 0.3052 0.068 Uiso 1 1 calc . . .
C14 C 0.0235(17) 0.5671(9) 0.3361(9) 0.063(3) Uani 1 1 d . . .
H14 H -0.0598 0.5946 0.2830 0.075 Uiso 1 1 calc . . .
C15 C 0.1882(17) 0.6516(9) 0.3975(10) 0.064(3) Uani 1 1 d . . .
H15 H 0.2199 0.7380 0.3876 0.077 Uiso 1 1 calc . . .
C16 C 0.3093(16) 0.6124(9) 0.4741(10) 0.065(3) Uani 1 1 d . . .
H16 H 0.4253 0.6717 0.5161 0.078 Uiso 1 1 calc . . .
C17 C 0.2641(15) 0.4876(9) 0.4908(9) 0.059(3) Uani 1 1 d . . .
H17 H 0.3481 0.4608 0.5441 0.071 Uiso 1 1 calc . . .
C18 C 0.244(2) 0.3406(18) 0.2168(17) 0.143(8) Uani 1 1 d . . .
H18A H 0.3189 0.3416 0.2951 0.171 Uiso 1 1 calc . . .
H18B H 0.2363 0.4275 0.2140 0.171 Uiso 1 1 calc . . .
C19 C 0.323(2) 0.3110(14) 0.1424(16) 0.124(7) Uani 1 1 d . . .
H19A H 0.4456 0.3158 0.1848 0.149 Uiso 1 1 calc . . .
H19B H 0.3247 0.3714 0.0898 0.149 Uiso 1 1 calc . . .
C20 C 0.208(2) 0.1749(11) 0.0779(12) 0.083(4) Uani 1 1 d . . .
H20A H 0.1496 0.1726 -0.0037 0.099 Uiso 1 1 calc . . .
H20B H 0.2785 0.1172 0.0869 0.099 Uiso 1 1 calc . . .
C21 C 0.077(2) 0.1392(11) 0.1320(14) 0.094(5) Uani 1 1 d . . .
H21A H -0.0421 0.0912 0.0740 0.112 Uiso 1 1 calc . . .
H21B H 0.1091 0.0836 0.1860 0.112 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
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'
N N 0.0061 0.0033 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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
N1 Pt N1 179.999(1) . 2_556 ?
N1 Pt C2 84.1(3) . 2_556 ?
N1 Pt C2 95.9(3) 2_556 2_556 ?
N1 Pt C2 95.9(3) . . ?
N1 Pt C2 84.1(3) 2_556 . ?
C2 Pt C2 179.998(1) 2_556 . ?
N1 Pt C1 102.2(3) . . ?
N1 Pt C1 77.8(3) 2_556 . ?
C2 Pt C1 99.7(3) 2_556 . ?
C2 Pt C1 80.3(3) . . ?
N1 Pt C1 77.8(3) . 2_556 ?
N1 Pt C1 102.2(3) 2_556 2_556 ?
C2 Pt C1 80.3(3) 2_556 2_556 ?
C2 Pt C1 99.7(3) . 2_556 ?
C1 Pt C1 180.0(4) . 2_556 ?
N1 Pt Mo 87.1(2) . . ?
N1 Pt Mo 92.9(2) 2_556 . ?
C2 Pt Mo 137.5(2) 2_556 . ?
C2 Pt Mo 42.5(2) . . ?
C1 Pt Mo 42.2(2) . . ?
C1 Pt Mo 137.8(2) 2_556 . ?
N1 Pt Mo 92.9(2) . 2_556 ?
N1 Pt Mo 87.1(2) 2_556 2_556 ?
C2 Pt Mo 42.5(2) 2_556 2_556 ?
C2 Pt Mo 137.5(2) . 2_556 ?
C1 Pt Mo 137.8(2) . 2_556 ?
C1 Pt Mo 42.2(2) 2_556 2_556 ?
Mo Pt Mo 180.00(3) . 2_556 ?
C3 Mo C2 82.0(4) . . ?
C3 Mo C1 85.3(4) . . ?
C2 Mo C1 113.4(4) . . ?
C3 Mo C5 145.1(4) . . ?
C2 Mo C5 128.7(4) . . ?
C1 Mo C5 94.5(4) . . ?
C3 Mo C6 144.9(4) . . ?
C2 Mo C6 97.2(4) . . ?
C1 Mo C6 125.7(4) . . ?
C5 Mo C6 34.9(4) . . ?
C3 Mo C4 109.1(4) . . ?
C2 Mo C4 151.8(4) . . ?
C1 Mo C4 93.7(4) . . ?
C5 Mo C4 36.0(4) . . ?
C6 Mo C4 58.5(4) . . ?
C3 Mo C7 109.6(4) . . ?
C2 Mo C7 93.9(4) . . ?
C1 Mo C7 150.7(4) . . ?
C5 Mo C7 58.6(3) . . ?
C6 Mo C7 35.2(3) . . ?
C4 Mo C7 58.0(4) . . ?
C3 Mo C8 93.3(4) . . ?
C2 Mo C8 122.5(4) . . ?
C1 Mo C8 123.3(4) . . ?
C5 Mo C8 57.8(3) . . ?
C6 Mo C8 57.3(3) . . ?
C4 Mo C8 34.1(3) . . ?
C7 Mo C8 34.3(3) . . ?
C3 Mo Pt 105.7(3) . . ?
C2 Mo Pt 59.4(3) . . ?
C1 Mo Pt 62.3(3) . . ?
C5 Mo Pt 105.1(3) . . ?
C6 Mo Pt 103.9(3) . . ?
C4 Mo Pt 135.5(3) . . ?
C7 Mo Pt 131.6(2) . . ?
C8 Mo Pt 160.8(2) . . ?
C18 O4 C21 105.6(12) . . ?
C11 N1 Pt 174.7(8) . . ?
C8 N2 C9 119.9(9) . . ?
C8 N2 C10 116.7(9) . . ?
C9 N2 C10 111.9(9) . . ?
O1 C1 Mo 172.0(9) . . ?
O1 C1 Pt 112.0(7) . . ?
Mo C1 Pt 75.5(3) . . ?
O2 C2 Mo 170.1(8) . . ?
O2 C2 Pt 111.7(7) . . ?
Mo C2 Pt 78.2(3) . . ?
O3 C3 Mo 177.2(10) . . ?
C8 C4 C5 108.1(10) . . ?
C8 C4 Mo 76.9(6) . . ?
C5 C4 Mo 70.9(6) . . ?
C8 C4 H4 126.0 . . ?
C5 C4 H4 126.0 . . ?
Mo C4 H4 118.1 . . ?
C6 C5 C4 107.2(9) . . ?
C6 C5 Mo 72.6(6) . . ?
C4 C5 Mo 73.1(5) . . ?
C6 C5 H5 126.4 . . ?
C4 C5 H5 126.4 . . ?
Mo C5 H5 119.8 . . ?
C5 C6 C7 109.1(9) . . ?
C5 C6 Mo 72.5(6) . . ?
C7 C6 Mo 73.8(5) . . ?
C5 C6 H6 125.4 . . ?
C7 C6 H6 125.4 . . ?
Mo C6 H6 120.0 . . ?
C6 C7 C8 107.7(8) . . ?
C6 C7 Mo 70.9(5) . . ?
C8 C7 Mo 76.3(5) . . ?
C6 C7 H7 126.2 . . ?
C8 C7 H7 126.2 . . ?
Mo C7 H7 118.5 . . ?
N2 C8 C4 125.5(10) . . ?
N2 C8 C7 126.9(9) . . ?
C4 C8 C7 107.6(9) . . ?
N2 C8 Mo 126.4(6) . . ?
C4 C8 Mo 69.1(6) . . ?
C7 C8 Mo 69.4(5) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 177.3(11) . . ?
C13 C12 C17 120.6(9) . . ?
C13 C12 C11 121.6(10) . . ?
C17 C12 C11 117.8(9) . . ?
C12 C13 C14 119.1(10) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C15 C14 C13 120.7(10) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 120.0(9) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 120.7(11) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 119.0(10) . . ?
C12 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
O4 C18 C19 111.2(12) . . ?
O4 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
O4 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 C20 105.4(12) . . ?
C18 C19 H19A 110.7 . . ?
C20 C19 H19A 110.7 . . ?
C18 C19 H19B 110.7 . . ?
C20 C19 H19B 110.7 . . ?
H19A C19 H19B 108.8 . . ?
C21 C20 C19 102.6(10) . . ?
C21 C20 H20A 111.3 . . ?
C19 C20 H20A 111.3 . . ?
C21 C20 H20B 111.3 . . ?
C19 C20 H20B 111.3 . . ?
H20A C20 H20B 109.2 . . ?
O4 C21 C20 108.0(10) . . ?
O4 C21 H21A 110.1 . . ?
C20 C21 H21A 110.1 . . ?
O4 C21 H21B 110.1 . . ?
C20 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
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
Pt N1 1.942(7) . ?
Pt N1 1.942(7) 2_556 ?
Pt C2 2.509(9) 2_556 ?
Pt C2 2.509(9) . ?
Pt C1 2.611(10) . ?
Pt C1 2.611(10) 2_556 ?
Pt Mo 2.854(3) . ?
Pt Mo 2.854(3) 2_556 ?
Mo C3 1.928(10) . ?
Mo C2 1.970(11) . ?
Mo C1 1.982(11) . ?
Mo C5 2.312(9) . ?
Mo C6 2.314(9) . ?
Mo C4 2.341(10) . ?
Mo C7 2.351(9) . ?
Mo C8 2.440(10) . ?
O1 C1 1.164(11) . ?
O2 C2 1.161(11) . ?
O3 C3 1.177(12) . ?
O4 C18 1.372(18) . ?
O4 C21 1.404(14) . ?
N1 C11 1.150(10) . ?
N2 C8 1.356(13) . ?
N2 C9 1.460(15) . ?
N2 C10 1.468(14) . ?
C4 C8 1.403(14) . ?
C4 C5 1.437(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.412(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.416(14) . ?
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 1.449(11) . ?
C12 C13 1.375(14) . ?
C12 C17 1.379(14) . ?
C13 C14 1.390(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.353(16) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(13) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.40(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.516(18) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.474(18) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
