#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:49:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179426 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/23/4332389.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_4332389
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         'C28 H18 Mo2 O6'
_chemical_formula_sum            'C28 H18 Mo2 O6'
_chemical_formula_weight         642.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.577(5)
_cell_length_b                   12.608(5)
_cell_length_c                   25.024(5)
_cell_measurement_reflns_used    16969
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2390.6(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    0.0860
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2732
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0271
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                1771
_reflns_number_total             2732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060318dsup1.cif
_cod_data_source_block           st912
_cod_original_sg_symbol_H-M      Pcab
_cod_database_code               4332389
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, 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
Mo Mo 0.51549(3) 0.005953(17) 0.063964(9) 0.01762(9) Uani 1 1 d
O1 O 0.8714(3) 0.08650(18) 0.01569(8) 0.0338(5) Uani 1 1 d
O2 O 0.4589(3) -0.23501(17) 0.03964(9) 0.0413(6) Uani 1 1 d
O3 O 0.8067(3) -0.10048(18) 0.13358(9) 0.0458(6) Uani 1 1 d
C1 C 0.7375(4) 0.0542(2) 0.02980(11) 0.0239(7) Uani 1 1 d
C2 C 0.4836(4) -0.1461(2) 0.04542(11) 0.0262(7) Uani 1 1 d
C3 C 0.6990(4) -0.0622(2) 0.10808(12) 0.0296(7) Uani 1 1 d
C4 C 0.4581(4) 0.1177(2) 0.13483(11) 0.0245(6) Uani 1 1 d
H4 H 0.5508 0.1347 0.1589 0.029 Uiso 1 1 calc
C5 C 0.4140(4) 0.1756(2) 0.08817(12) 0.0275(7) Uani 1 1 d
H5 H 0.4708 0.2380 0.0757 0.033 Uiso 1 1 calc
C6 C 0.2705(4) 0.1238(2) 0.06362(11) 0.0252(7) Uani 1 1 d
H6 H 0.2136 0.1454 0.0316 0.030 Uiso 1 1 calc
C7 C 0.2253(4) 0.0340(2) 0.09490(11) 0.0237(6) Uani 1 1 d
H7 H 0.1335 -0.0150 0.0871 0.028 Uiso 1 1 calc
C8 C 0.3402(4) 0.0293(2) 0.13981(11) 0.0230(6) Uani 1 1 d
C9 C 0.3309(4) -0.0473(2) 0.18456(11) 0.0229(6) Uani 1 1 d
C10 C 0.2415(4) -0.1426(2) 0.17891(11) 0.0322(7) Uani 1 1 d
H10 H 0.1876 -0.1595 0.1457 0.039 Uiso 1 1 calc
C11 C 0.2297(4) -0.2140(3) 0.22121(13) 0.0378(8) Uani 1 1 d
H11 H 0.1678 -0.2790 0.2170 0.045 Uiso 1 1 calc
C12 C 0.3082(5) -0.1899(3) 0.26905(13) 0.0410(9) Uani 1 1 d
H12 H 0.2999 -0.2384 0.2980 0.049 Uiso 1 1 calc
C13 C 0.3991(5) -0.0958(3) 0.27566(12) 0.0408(9) Uani 1 1 d
H13 H 0.4543 -0.0803 0.3088 0.049 Uiso 1 1 calc
C14 C 0.4098(4) -0.0237(3) 0.23361(12) 0.0320(7) Uani 1 1 d
H14 H 0.4708 0.0414 0.2383 0.038 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'
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'
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
C3 Mo C1 77.10(12) .
C3 Mo C2 78.25(12) .
C1 Mo C2 107.37(12) .
C3 Mo C4 88.21(11) .
C1 Mo C4 107.71(11) .
C2 Mo C4 138.24(11) .
C3 Mo C8 90.06(11) .
C1 Mo C8 142.59(11) .
C2 Mo C8 104.03(11) .
C4 Mo C8 35.97(9) .
C3 Mo C5 118.84(11) .
C1 Mo C5 96.29(11) .
C2 Mo C5 153.83(11) .
C4 Mo C5 35.40(9) .
C8 Mo C5 59.34(10) .
C3 Mo C7 122.62(11) .
C1 Mo C7 152.48(11) .
C2 Mo C7 96.19(11) .
C4 Mo C7 58.67(10) .
C8 Mo C7 35.30(9) .
C5 Mo C7 58.27(10) .
C3 Mo C6 145.55(11) .
C1 Mo C6 117.98(11) .
C2 Mo C6 120.46(11) .
C4 Mo C6 58.25(10) .
C8 Mo C6 58.67(9) .
C5 Mo C6 34.66(10) .
C7 Mo C6 34.86(9) .
C3 Mo Mo 126.07(9) 5_655
C1 Mo Mo 69.31(8) 5_655
C2 Mo Mo 73.34(8) 5_655
C4 Mo Mo 141.33(7) 5_655
C8 Mo Mo 140.72(7) 5_655
C5 Mo Mo 105.97(7) 5_655
C7 Mo Mo 105.43(7) 5_655
C6 Mo Mo 88.20(7) 5_655
O1 C1 Mo 172.1(3) .
O2 C2 Mo 173.4(3) .
O3 C3 Mo 179.1(3) .
C5 C4 C8 109.0(3) .
C5 C4 Mo 74.08(16) .
C8 C4 Mo 73.10(16) .
C5 C4 H4 125.5 .
C8 C4 H4 125.5 .
Mo C4 H4 119.1 .
C6 C5 C4 107.6(3) .
C6 C5 Mo 73.66(16) .
C4 C5 Mo 70.52(15) .
C6 C5 H5 126.2 .
C4 C5 H5 126.2 .
Mo C5 H5 121.4 .
C5 C6 C7 108.4(2) .
C5 C6 Mo 71.68(16) .
C7 C6 Mo 71.78(16) .
C5 C6 H6 125.8 .
C7 C6 H6 125.8 .
Mo C6 H6 122.4 .
C6 C7 C8 108.7(3) .
C6 C7 Mo 73.37(16) .
C8 C7 Mo 71.49(16) .
C6 C7 H7 125.6 .
C8 C7 H7 125.6 .
Mo C7 H7 121.2 .
C7 C8 C4 106.3(3) .
C7 C8 C9 126.5(3) .
C4 C8 C9 127.0(3) .
C7 C8 Mo 73.21(16) .
C4 C8 Mo 70.92(16) .
C9 C8 Mo 124.04(18) .
C10 C9 C14 118.9(3) .
C10 C9 C8 120.8(3) .
C14 C9 C8 120.4(3) .
C9 C10 C11 120.9(3) .
C9 C10 H10 119.5 .
C11 C10 H10 119.5 .
C12 C11 C10 119.5(3) .
C12 C11 H11 120.2 .
C10 C11 H11 120.2 .
C11 C12 C13 120.7(3) .
C11 C12 H12 119.6 .
C13 C12 H12 119.6 .
C12 C13 C14 119.9(3) .
C12 C13 H13 120.0 .
C14 C13 H13 120.0 .
C13 C14 C9 120.0(3) .
C13 C14 H14 120.0 .
C9 C14 H14 120.0 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo C3 1.972(3) .
Mo C1 1.983(3) .
Mo C2 1.987(3) .
Mo C4 2.306(3) .
Mo C8 2.335(3) .
Mo C5 2.353(3) .
Mo C7 2.357(3) .
Mo C6 2.378(3) .
Mo Mo 3.2134(8) 5_655
O1 C1 1.149(3) .
O2 C2 1.146(3) .
O3 C3 1.143(3) .
C4 C5 1.417(4) .
C4 C8 1.433(4) .
C4 H4 0.9500 .
C5 C6 1.409(4) .
C5 H5 0.9500 .
C6 C7 1.418(4) .
C6 H6 0.9500 .
C7 C8 1.423(4) .
C7 H7 0.9500 .
C8 C9 1.480(4) .
C9 C10 1.387(4) .
C9 C14 1.397(4) .
C10 C11 1.392(4) .
C10 H10 0.9500 .
C11 C12 1.371(5) .
C11 H11 0.9500 .
C12 C13 1.382(5) .
C12 H12 0.9500 .
C13 C14 1.392(4) .
C13 H13 0.9500 .
C14 H14 0.9500 .
