#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:12:02 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178940 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/69/4116906.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_4116906
loop_
_publ_author_name
'F. Albert Cotton'
'Lee M. Daniels'
'Isabelle Guimet'
'Robert W. Henning'
'Glenn T. Jordan'
'Chun Lin'
'Carlos A. Murillo'
'Arthur J. Schultz'
_publ_section_title
;
 Compounds with Two Metal-Metal Multiple Bonds: New Ways of Making
 Doublets into Cyclic Quartets
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12531
_journal_page_last               12538
_journal_paper_doi               10.1021/ja982425f
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C60 H52 Cl4 F8 Mo4 N8 O2'
_chemical_formula_weight         1594.66
_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
_cell_angle_alpha                67.930(10)
_cell_angle_beta                 70.12(2)
_cell_angle_gamma                76.15(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0030(10)
_cell_length_b                   13.027(3)
_cell_length_c                   14.099(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     1588.0(6)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        PROCOR
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6373
_diffrn_reflns_theta_max         22.59
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'reddish yellow'
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       tablet
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.117
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         3655
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.127
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         0.195
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0670P)²+5.7200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1317
_refine_ls_wR_factor_obs         0.1243
_reflns_number_observed          3335
_reflns_number_total             3658
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja982425f_7.cif
_cod_data_source_block           CMPD_4c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+5.7200P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+5.7200P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1588.0(5)
_cod_database_code               4116906
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.42567(6) 0.03481(4) 0.64201(4) 0.0296(2) Uani 1 d . .
Mo2 Mo 0.38440(5) -0.11368(4) 0.63383(4) 0.0290(2) Uani 1 d . .
Cl1 Cl 0.6804(2) 0.05952(13) 0.53690(12) 0.0349(4) Uani 1 d . .
Cl2 Cl 0.3807(2) 0.18415(12) 0.47615(12) 0.0335(4) Uani 1 d . .
F1 F 0.0399(7) 0.4002(4) 0.9173(4) 0.084(2) Uani 1 d . .
F2 F -0.2079(5) -0.3585(4) 0.7448(4) 0.0698(14) Uani 1 d . .
F3 F 0.7347(6) 0.1442(6) 0.9595(4) 0.086(2) Uani 1 d . .
F4 F 0.3359(5) -0.6512(3) 0.9776(4) 0.0639(13) Uani 1 d . .
N1 N 0.2106(6) 0.0720(4) 0.7232(4) 0.0369(14) Uani 1 d . .
N2 N 0.1663(5) -0.0858(4) 0.7107(4) 0.0330(13) Uani 1 d . .
N3 N 0.4955(6) -0.0533(4) 0.7800(4) 0.0324(13) Uani 1 d . .
N4 N 0.4413(5) -0.2120(4) 0.7749(4) 0.0306(12) Uani 1 d . .
C1 C 0.1173(7) 0.0049(6) 0.7387(5) 0.036(2) Uani 1 d . .
H1A H 0.0188(7) 0.0221(6) 0.7689(5) 0.044 Uiso 1 calc R .
C2 C 0.4895(7) -0.1624(6) 0.8215(5) 0.033(2) Uani 1 d . .
H2A H 0.5191(7) -0.2043(6) 0.8832(5) 0.040 Uiso 1 calc R .
C11 C 0.1600(7) 0.1585(5) 0.7712(5) 0.038(2) Uani 1 d . .
C12 C 0.2069(10) 0.2641(7) 0.7172(7) 0.062(2) Uani 1 d . .
H12A H 0.2666(10) 0.2807(7) 0.6469(7) 0.075 Uiso 1 calc R .
C13 C 0.1639(11) 0.3442(7) 0.7688(7) 0.070(3) Uani 1 d . .
H13A H 0.1950(11) 0.4151(7) 0.7336(7) 0.084 Uiso 1 calc R .
C14 C 0.0781(9) 0.3197(7) 0.8689(7) 0.055(2) Uani 1 d . .
C15 C 0.0327(9) 0.2202(7) 0.9223(6) 0.055(2) Uani 1 d . .
H15A H -0.0272(9) 0.2057(7) 0.9925(6) 0.066 Uiso 1 calc R .
C16 C 0.0740(8) 0.1377(6) 0.8741(6) 0.047(2) Uani 1 d . .
H16A H 0.0428(8) 0.0672(6) 0.9122(6) 0.056 Uiso 1 calc R .
C21 C 0.0644(7) -0.1539(5) 0.7208(5) 0.033(2) Uani 1 d . .
C22 C 0.0650(7) -0.2619(6) 0.7907(6) 0.044(2) Uani 1 d . .
H22A H 0.1293(7) -0.2888(6) 0.8328(6) 0.052 Uiso 1 calc R .
C23 C -0.0260(8) -0.3301(6) 0.7998(7) 0.054(2) Uani 1 d . .
H23A H -0.0261(8) -0.4032(6) 0.8483(7) 0.064 Uiso 1 calc R .
C24 C -0.1166(8) -0.2901(6) 0.7372(6) 0.045(2) Uani 1 d . .
C25 C -0.1223(8) -0.1840(7) 0.6670(6) 0.050(2) Uani 1 d . .
H25A H -0.1872(8) -0.1580(7) 0.6253(6) 0.060 Uiso 1 calc R .
C26 C -0.0287(7) -0.1161(6) 0.6594(6) 0.043(2) Uani 1 d . .
H26A H -0.0293(7) -0.0429(6) 0.6112(6) 0.051 Uiso 1 calc R .
C31 C 0.5607(7) -0.0029(6) 0.8247(5) 0.033(2) Uani 1 d . .
C32 C 0.6715(8) -0.0604(7) 0.8701(6) 0.050(2) Uani 1 d . .
H32A H 0.7081(8) -0.1337(7) 0.8695(6) 0.060 Uiso 1 calc R .
C33 C 0.7289(8) -0.0109(8) 0.9162(6) 0.052(2) Uani 1 d . .
H33A H 0.8013(8) -0.0506(8) 0.9496(6) 0.063 Uiso 1 calc R .
C34 C 0.6776(10) 0.0969(9) 0.9117(7) 0.063(2) Uani 1 d . .
C35 C 0.5732(9) 0.1571(8) 0.8644(8) 0.067(2) Uani 1 d . .
H35A H 0.5419(9) 0.2323(8) 0.8605(8) 0.080 Uiso 1 calc R .
C36 C 0.5148(9) 0.1050(7) 0.8227(6) 0.053(2) Uani 1 d . .
H36A H 0.4405(9) 0.1451(7) 0.7914(6) 0.063 Uiso 1 calc R .
C41 C 0.4183(6) -0.3259(5) 0.8286(5) 0.0285(14) Uani 1 d . .
C42 C 0.4525(8) -0.3973(6) 0.7706(5) 0.045(2) Uani 1 d . .
H42A H 0.4966(8) -0.3714(6) 0.6970(5) 0.054 Uiso 1 calc R .
C43 C 0.4232(9) -0.5077(6) 0.8192(6) 0.054(2) Uani 1 d . .
H43A H 0.4444(9) -0.5564(6) 0.7794(6) 0.065 Uiso 1 calc R .
C44 C 0.3612(8) -0.5424(6) 0.9285(6) 0.047(2) Uani 1 d . .
C45 C 0.3267(7) -0.4740(6) 0.9886(5) 0.041(2) Uani 1 d . .
H45A H 0.2858(7) -0.5009(6) 1.0626(5) 0.049 Uiso 1 calc R .
C46 C 0.3531(6) -0.3637(5) 0.9382(5) 0.034(2) Uani 1 d . .
H46A H 0.3271(6) -0.3144(5) 0.9778(5) 0.041 Uiso 1 calc R .
C5S C 0.9009(53) -0.6970(42) 0.5820(37) 0.254(22) Uiso 0.69(3) d PD 1
C1S C 0.7951(39) -0.6536(31) 0.4875(28) 0.193(15) Uiso 0.69(3) d PD 1
C2S C 0.6141(59) -0.5847(52) 0.5046(47) 0.350(32) Uiso 0.69(3) d PD 1
C3S C 0.6508(33) -0.5984(27) 0.6170(26) 0.168(12) Uiso 0.69(3) d PD 1
C4S C 0.8082(46) -0.6273(46) 0.6531(37) 0.231(19) Uiso 0.69(3) d PD 1
C5S' C 0.8252(90) -0.5461(91) 0.6123(72) 0.213(37) Uiso 0.31(3) d PD 2
C1S' C 0.7359(82) -0.5349(56) 0.5375(60) 0.174(29) Uiso 0.31(3) d PD 2
C2S' C 0.6665(56) -0.6484(45) 0.5459(45) 0.128(19) Uiso 0.31(3) d PD 2
C3S' C 0.8280(50) -0.7188(40) 0.5773(38) 0.111(17) Uiso 0.31(3) d PD 2
C4S' C 0.8683(88) -0.5796(57) 0.5045(56) 0.195(34) Uiso 0.31(3) d PD 2
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mo1 N3 95.8(2) . . y
N1 Mo1 Mo2 92.1(2) . . y
N3 Mo1 Mo2 92.1(2) . . y
N1 Mo1 Cl1 160.3(2) . . y
N3 Mo1 Cl1 89.04(14) . . y
Mo2 Mo1 Cl1 106.90(5) . . y
N1 Mo1 Cl2 88.62(14) . . y
N3 Mo1 Cl2 162.7(2) . . y
Mo2 Mo1 Cl2 104.41(5) . . y
Cl1 Mo1 Cl2 81.50(5) . . y
N2 Mo2 N4 94.5(2) . . y
N2 Mo2 Mo1 92.3(2) . . y
N4 Mo2 Mo1 92.4(2) . . y
N2 Mo2 Cl1 88.44(15) . 2_656 y
N4 Mo2 Cl1 161.0(2) . 2_656 y
Mo1 Mo2 Cl1 106.30(5) . 2_656 y
N2 Mo2 Cl2 162.8(2) . 2_656 y
N4 Mo2 Cl2 90.74(15) . 2_656 y
Mo1 Mo2 Cl2 103.86(5) . 2_656 y
Cl1 Mo2 Cl2 81.45(6) 2_656 2_656 y
Mo1 Cl1 Mo2 90.72(5) . 2_656 y
Mo2 Cl2 Mo1 90.15(5) 2_656 . y
C1 N1 C11 117.8(6) . . ?
C1 N1 Mo1 117.9(5) . . ?
C11 N1 Mo1 124.0(4) . . ?
C1 N2 C21 118.4(5) . . ?
C1 N2 Mo2 118.9(4) . . ?
C21 N2 Mo2 122.1(4) . . ?
C2 N3 C31 118.7(5) . . ?
C2 N3 Mo1 118.0(4) . . ?
C31 N3 Mo1 123.1(4) . . ?
C2 N4 C41 118.0(5) . . ?
C2 N4 Mo2 118.0(4) . . ?
C41 N4 Mo2 123.6(4) . . ?
N2 C1 N1 118.6(6) . . ?
N3 C2 N4 119.3(6) . . ?
C16 C11 C12 118.2(7) . . ?
C16 C11 N1 120.9(6) . . ?
C12 C11 N1 120.6(6) . . ?
C13 C12 C11 119.4(8) . . ?
C14 C13 C12 119.8(8) . . ?
C15 C14 C13 122.3(8) . . ?
C15 C14 F1 119.8(8) . . ?
C13 C14 F1 117.9(8) . . ?
C14 C15 C16 119.8(8) . . ?
C11 C16 C15 120.6(7) . . ?
C26 C21 C22 118.9(6) . . ?
C26 C21 N2 121.7(6) . . ?
C22 C21 N2 119.4(6) . . ?
C23 C22 C21 121.2(6) . . ?
C24 C23 C22 118.4(6) . . ?
C23 C24 C25 123.0(7) . . ?
C23 C24 F2 119.0(6) . . ?
C25 C24 F2 118.0(6) . . ?
C24 C25 C26 117.4(6) . . ?
C21 C26 C25 121.1(6) . . ?
C36 C31 C32 118.0(7) . . ?
C36 C31 N3 120.0(6) . . ?
C32 C31 N3 122.0(6) . . ?
C33 C32 C31 120.7(7) . . ?
C34 C33 C32 118.1(8) . . ?
C35 C34 C33 122.9(8) . . ?
C35 C34 F3 119.9(9) . . ?
C33 C34 F3 117.2(9) . . ?
C34 C35 C36 117.9(8) . . ?
C31 C36 C35 122.3(8) . . ?
C42 C41 C46 119.8(6) . . ?
C42 C41 N4 119.3(6) . . ?
C46 C41 N4 120.7(6) . . ?
C41 C42 C43 121.1(7) . . ?
C44 C43 C42 117.2(8) . . ?
C45 C44 F4 118.9(7) . . ?
C45 C44 C43 123.2(7) . . ?
F4 C44 C43 117.8(8) . . ?
C44 C45 C46 118.6(6) . . ?
C45 C46 C41 120.0(7) . . ?
C4S C5S C1S 97.8(31) . . ?
C2S C1S C5S 126.9(33) . . ?
C3S C2S C1S 76.4(28) . . ?
C2S C3S C4S 133.5(31) . . ?
C5S C4S C3S 99.9(32) . . ?
C1S' C5S' C4S' 48.8(41) . . ?
C5S' C1S' C2S' 121.0(59) . . ?
C1S' C2S' C3S' 81.3(36) . . ?
C2S' C3S' C4S' 77.2(38) . . ?
C5S' C4S' C3S' 92.7(54) . . ?
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
Mo1 N1 2.101(5) . y
Mo1 N3 2.110(5) . y
Mo1 Mo2 2.1231(9) . y
Mo1 Cl1 2.502(2) . y
Mo1 Cl2 2.517(2) . y
Mo1 Mo2 3.5633(12) 2_656 y
Mo2 N2 2.092(5) . y
Mo2 N4 2.104(5) . y
Mo2 Cl1 2.506(2) 2_656 y
Mo2 Cl2 2.516(2) 2_656 y
Cl1 Mo2 2.506(2) 2_656 y
Cl2 Mo2 2.516(2) 2_656 y
F1 C14 1.371(10) . ?
F2 C24 1.375(8) . ?
F3 C34 1.379(10) . ?
F4 C44 1.366(8) . ?
N1 C1 1.338(9) . ?
N1 C11 1.432(9) . ?
N2 C1 1.316(9) . ?
N2 C21 1.445(9) . ?
N3 C2 1.326(8) . ?
N3 C31 1.432(9) . ?
N4 C2 1.327(8) . ?
N4 C41 1.425(8) . ?
C11 C16 1.373(10) . ?
C11 C12 1.405(10) . ?
C12 C13 1.395(12) . ?
C13 C14 1.342(12) . ?
C14 C15 1.330(11) . ?
C15 C16 1.391(11) . ?
C21 C26 1.367(9) . ?
C21 C22 1.382(9) . ?
C22 C23 1.363(10) . ?
C23 C24 1.357(10) . ?
C24 C25 1.366(10) . ?
C25 C26 1.389(10) . ?
C31 C36 1.364(11) . ?
C31 C32 1.387(10) . ?
C32 C33 1.383(11) . ?
C33 C34 1.360(13) . ?
C34 C35 1.356(13) . ?
C35 C36 1.368(12) . ?
C41 C42 1.370(10) . ?
C41 C46 1.397(9) . ?
C42 C43 1.396(10) . ?
C43 C44 1.388(11) . ?
C44 C45 1.360(11) . ?
C45 C46 1.388(9) . ?
C5S C4S 1.53(5) . ?
C5S C1S 1.82(5) . ?
C1S C2S 1.80(5) . ?
C2S C3S 1.68(5) . ?
C3S C4S 1.73(4) . ?
C5S' C1S' 1.55(6) . ?
C5S' C4S' 1.63(7) . ?
C1S' C2S' 1.73(6) . ?
C2S' C3S' 1.77(6) . ?
C3S' C4S' 1.78(6) . ?
