#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:49:31 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178918 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/47/4114703.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_4114703
loop_
_publ_author_name
'F. Albert Cotton'
'Lee M. Daniels'
'Carlos A. Murillo'
'J. Garrett Slaton'
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, P.O. Box 30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 A Pseudo-Jahn-Teller Distortion in an Mo2(μ2-O)2 Ring Having the
 Shortest MoIV-MoIV Double Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2878
_journal_page_last               2879
_journal_paper_doi               10.1021/ja025713r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C60 H60 Mo2 N8 O10, 2C H2 Cl2'
_chemical_formula_sum            'C62 H64 Cl4 Mo2 N8 O10'
_chemical_formula_weight         1414.89
_chemical_name_common
;
tetrakis(anisylformamidinato)-bis(oxo)dimolybdenum(IV)
;
_chemical_name_systematic
;
 trans-bis-η²-(N,N'-di-(p-anisylformamidinato)
-bis-μ₂-oxobis(μ₂-N,N'-di-
(p-anisylformamidinato)dimolybdenum(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.1360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2805(7)
_cell_length_b                   10.3291(5)
_cell_length_c                   22.9583(12)
_cell_measurement_reflns_used    298
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.16
_cell_volume                     3147.1(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2001)'
_computing_data_collection       'SMART (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 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      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19042
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.538
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0453
_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)+(0.0598P)²+4.1334P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                5666
_reflns_number_total             7153
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja025713r_s1_1.cif
_cod_data_source_block           2
_cod_database_code               4114703
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Mo1 Mo 0.52614(2) 0.05655(3) 0.958952(11) 0.02939(10) Uani 1 1 d . . .
Cl1 Cl 0.11419(18) 0.9807(2) 0.95503(10) 0.1222(7) Uani 1 1 d . A .
Cl2A Cl 0.1461(4) 0.8106(3) 0.86140(13) 0.1845(17) Uani 0.879(4) 1 d P A 1
Cl2B Cl 0.168(3) 0.939(2) 0.8323(11) 0.1845(17) Uani 0.121(4) 1 d P A 2
O1 O 0.56928(16) 0.0926(2) 1.03936(9) 0.0316(5) Uani 1 1 d . . .
O2 O 0.4699(3) -0.2452(3) 0.67134(11) 0.0586(8) Uani 1 1 d . . .
O3 O 0.8803(3) 0.6072(3) 0.99078(13) 0.0674(9) Uani 1 1 d . . .
O4 O 0.3062(2) 0.5866(3) 0.81147(15) 0.0716(10) Uani 1 1 d . . .
O5 O 0.8773(2) -0.1214(3) 0.75257(11) 0.0527(7) Uani 1 1 d . . .
N1 N 0.5278(2) 0.0783(3) 0.86426(11) 0.0333(6) Uani 1 1 d . . .
N2 N 0.6143(2) 0.2122(3) 0.92194(11) 0.0332(6) Uani 1 1 d . . .
N3 N 0.4035(2) 0.1852(3) 0.96601(11) 0.0338(6) Uani 1 1 d . . .
N4 N 0.6460(2) -0.0796(3) 0.95047(11) 0.0327(6) Uani 1 1 d . . .
C1 C 0.5921(2) 0.1755(3) 0.86771(13) 0.0325(6) Uani 1 1 d . . .
H1A H 0.6192 0.2143 0.8353 0.039 Uiso 1 1 calc R . .
C2 C 0.5099(2) 0.0062(3) 0.81252(13) 0.0336(7) Uani 1 1 d . . .
C3 C 0.5449(3) 0.0425(4) 0.75800(15) 0.0488(9) Uani 1 1 d . . .
H3A H 0.5768 0.1219 0.7539 0.059 Uiso 1 1 calc R . .
C4 C 0.5324(4) -0.0382(4) 0.71017(16) 0.0554(11) Uani 1 1 d . . .
H4B H 0.5560 -0.0122 0.6744 0.066 Uiso 1 1 calc R . .
C5 C 0.4852(3) -0.1572(4) 0.71495(15) 0.0459(9) Uani 1 1 d . . .
C6 C 0.4476(3) -0.1922(4) 0.76892(15) 0.0428(8) Uani 1 1 d . . .
H6A H 0.4141 -0.2706 0.7727 0.051 Uiso 1 1 calc R . .
C7 C 0.4598(3) -0.1113(4) 0.81664(14) 0.0388(7) Uani 1 1 d . . .
H7A H 0.4340 -0.1359 0.8521 0.047 Uiso 1 1 calc R . .
C8 C 0.4976(5) -0.2060(5) 0.61409(18) 0.0876(19) Uani 1 1 d . . .
H8A H 0.4838 -0.2752 0.5870 0.131 Uiso 1 1 calc R . .
H8B H 0.5681 -0.1857 0.6146 0.131 Uiso 1 1 calc R . .
H8C H 0.4593 -0.1310 0.6023 0.131 Uiso 1 1 calc R . .
C9 C 0.6816(2) 0.3152(3) 0.93620(14) 0.0336(7) Uani 1 1 d . . .
C10 C 0.7160(3) 0.4040(4) 0.89606(16) 0.0458(9) Uani 1 1 d . . .
H10A H 0.6942 0.3977 0.8572 0.055 Uiso 1 1 calc R . .
C11 C 0.7819(3) 0.5012(4) 0.91302(16) 0.0459(8) Uani 1 1 d . . .
H11A H 0.8039 0.5599 0.8855 0.055 Uiso 1 1 calc R . .
C12 C 0.8153(3) 0.5121(4) 0.96984(17) 0.0455(8) Uani 1 1 d . . .
C13 C 0.7819(4) 0.4247(5) 1.01028(18) 0.0694(15) Uani 1 1 d . . .
H13A H 0.8053 0.4303 1.0489 0.083 Uiso 1 1 calc R . .
C14 C 0.7142(4) 0.3292(5) 0.99392(16) 0.0606(12) Uani 1 1 d . . .
H14A H 0.6901 0.2734 1.0220 0.073 Uiso 1 1 calc R . .
C15 C 0.9361(3) 0.6781(4) 0.9505(2) 0.0603(11) Uani 1 1 d . . .
H15A H 0.9778 0.7404 0.9710 0.090 Uiso 1 1 calc R . .
H15B H 0.8907 0.7222 0.9237 0.090 Uiso 1 1 calc R . .
H15C H 0.9778 0.6201 0.9293 0.090 Uiso 1 1 calc R . .
C16 C 0.3433(2) 0.1733(3) 1.01082(13) 0.0329(6) Uani 1 1 d . . .
H16A H 0.2918 0.2333 1.0150 0.039 Uiso 1 1 calc R . .
C17 C 0.3783(2) 0.2880(3) 0.92603(13) 0.0330(7) Uani 1 1 d . . .
C18 C 0.4283(3) 0.4052(4) 0.92932(17) 0.0472(9) Uani 1 1 d . . .
H18A H 0.4793 0.4184 0.9576 0.057 Uiso 1 1 calc R . .
C19 C 0.4021(3) 0.5034(4) 0.8902(2) 0.0547(10) Uani 1 1 d . . .
H19A H 0.4354 0.5826 0.8925 0.066 Uiso 1 1 calc R . .
C20 C 0.3266(3) 0.4841(4) 0.84779(16) 0.0459(9) Uani 1 1 d . . .
C21 C 0.2775(4) 0.3678(4) 0.84499(19) 0.0620(12) Uani 1 1 d . . .
H21A H 0.2264 0.3541 0.8169 0.074 Uiso 1 1 calc R . .
C22 C 0.3041(4) 0.2707(4) 0.88411(19) 0.0597(12) Uani 1 1 d . . .
H22A H 0.2706 0.1917 0.8817 0.072 Uiso 1 1 calc R . .
C23 C 0.2328(5) 0.5689(6) 0.7661(3) 0.112(3) Uani 1 1 d . . .
H23A H 0.2257 0.6474 0.7439 0.169 Uiso 1 1 calc R . .
H23B H 0.1694 0.5473 0.7824 0.169 Uiso 1 1 calc R . .
H23C H 0.2533 0.5000 0.7411 0.169 Uiso 1 1 calc R . .
C24 C 0.7099(2) -0.0891(3) 0.90094(13) 0.0323(7) Uani 1 1 d . . .
C25 C 0.7835(3) 0.0013(4) 0.89174(14) 0.0379(7) Uani 1 1 d . . .
H25A H 0.7946 0.0677 0.9186 0.046 Uiso 1 1 calc R . .
C26 C 0.8419(3) -0.0056(4) 0.84218(15) 0.0404(8) Uani 1 1 d . . .
H26A H 0.8913 0.0560 0.8359 0.048 Uiso 1 1 calc R . .
C27 C 0.8249(3) -0.1058(4) 0.80261(14) 0.0393(7) Uani 1 1 d . . .
C28 C 0.7515(3) -0.1967(4) 0.81196(15) 0.0416(8) Uani 1 1 d . . .
H28A H 0.7406 -0.2636 0.7853 0.050 Uiso 1 1 calc R . .
C29 C 0.6938(3) -0.1890(3) 0.86079(14) 0.0385(7) Uani 1 1 d . . .
H29A H 0.6441 -0.2505 0.8668 0.046 Uiso 1 1 calc R . .
C30 C 0.9531(4) -0.0284(6) 0.7412(2) 0.0835(18) Uani 1 1 d . . .
H30A H 0.9841 -0.0495 0.7053 0.125 Uiso 1 1 calc R . .
H30B H 1.0032 -0.0291 0.7725 0.125 Uiso 1 1 calc R . .
H30C H 0.9233 0.0561 0.7382 0.125 Uiso 1 1 calc R . .
C31 C 0.1871(7) 0.9305(11) 0.8994(5) 0.169(4) Uani 1 1 d . . .
H31A H 0.1961 1.0032 0.8734 0.203 Uiso 1 1 calc R A 1
H31B H 0.2531 0.9078 0.9158 0.203 Uiso 1 1 calc R A 1
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'
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
O1 Mo1 O1 107.08(7) . 3_657 y
O1 Mo1 N3 90.43(10) . . ?
O1 Mo1 N3 89.55(10) 3_657 . ?
N3 Mo1 N4 177.65(11) . . ?
O1 Mo1 N2 94.87(10) . . ?
O1 Mo1 N2 158.04(9) 3_657 . ?
N3 Mo1 N2 89.59(10) . . ?
N4 Mo1 N2 92.11(10) . . ?
O1 Mo1 N1 155.36(10) . . ?
O1 Mo1 N1 97.38(9) 3_657 . ?
N3 Mo1 N1 92.76(10) . . ?
N4 Mo1 N1 86.66(10) . . ?
N2 Mo1 N1 60.75(10) . . y
O1 Mo1 Mo1 54.48(7) . 3_657 ?
O1 Mo1 Mo1 52.60(6) 3_657 3_657 ?
N3 Mo1 Mo1 89.97(7) . 3_657 ?
N4 Mo1 Mo1 89.39(7) . 3_657 ?
N2 Mo1 Mo1 149.34(7) . 3_657 ?
N1 Mo1 Mo1 149.85(7) . 3_657 ?
O1 Mo1 C1 125.12(10) . . ?
O1 Mo1 C1 127.71(9) 3_657 . ?
N3 Mo1 C1 92.78(10) . . ?
N4 Mo1 C1 87.87(10) . . ?
N2 Mo1 C1 30.48(10) . . ?
N1 Mo1 C1 30.33(10) . . ?
Mo1 Mo1 C1 177.23(7) 3_657 . ?
Mo1 O1 Mo1 72.93(7) . 3_657 y
C5 O2 C8 116.7(3) . . ?
C12 O3 C15 118.5(3) . . ?
C20 O4 C23 117.7(4) . . ?
C27 O5 C30 117.3(3) . . ?
C1 N1 C2 122.6(3) . . ?
C1 N1 Mo1 92.80(19) . . ?
C2 N1 Mo1 140.7(2) . . ?
C1 N2 C9 123.2(3) . . ?
C1 N2 Mo1 92.9(2) . . ?
C9 N2 Mo1 143.7(2) . . ?
C16 N3 C17 115.4(3) . . ?
C16 N3 Mo1 119.2(2) . . ?
C17 N3 Mo1 125.34(19) . . ?
C16 N4 C24 115.3(3) 3_657 . ?
C16 N4 Mo1 118.9(2) 3_657 . ?
C24 N4 Mo1 125.2(2) . . ?
N1 C1 N2 113.3(3) . . ?
N1 C1 Mo1 56.87(16) . . ?
N2 C1 Mo1 56.61(16) . . ?
C7 C2 C3 118.0(3) . . ?
C7 C2 N1 117.9(3) . . ?
C3 C2 N1 124.0(3) . . ?
C4 C3 C2 120.9(3) . . ?
C3 C4 C5 120.8(3) . . ?
O2 C5 C4 126.1(3) . . ?
O2 C5 C6 115.4(3) . . ?
C4 C5 C6 118.5(3) . . ?
C7 C6 C5 120.6(3) . . ?
C6 C7 C2 121.1(3) . . ?
C14 C9 C10 117.8(3) . . ?
C14 C9 N2 118.0(3) . . ?
C10 C9 N2 124.1(3) . . ?
C11 C10 C9 120.9(3) . . ?
C12 C11 C10 120.6(3) . . ?
C11 C12 C13 119.2(4) . . ?
C11 C12 O3 124.5(4) . . ?
C13 C12 O3 116.3(4) . . ?
C14 C13 C12 120.5(4) . . ?
C13 C14 C9 120.9(4) . . ?
N4 C16 N3 122.4(3) 3_657 . ?
C22 C17 C18 119.1(3) . . ?
C22 C17 N3 120.0(3) . . ?
C18 C17 N3 120.9(3) . . ?
C17 C18 C19 119.7(3) . . ?
C20 C19 C18 120.4(4) . . ?
C21 C20 O4 124.6(4) . . ?
C21 C20 C19 119.4(3) . . ?
O4 C20 C19 116.0(4) . . ?
C20 C21 C22 119.8(4) . . ?
C17 C22 C21 121.6(4) . . ?
C25 C24 C29 119.6(3) . . ?
C25 C24 N4 121.0(3) . . ?
C29 C24 N4 119.3(3) . . ?
C24 C25 C26 120.5(3) . . ?
C27 C26 C25 119.2(3) . . ?
O5 C27 C28 115.7(3) . . ?
O5 C27 C26 124.0(3) . . ?
C28 C27 C26 120.3(3) . . ?
C27 C28 C29 120.3(3) . . ?
C28 C29 C24 120.2(3) . . ?
Cl2B C31 Cl2A 57.4(9) . . ?
Cl2B C31 Cl1 130.4(14) . . ?
Cl2A C31 Cl1 116.8(6) . . ?
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 O1 1.948(2) . y
Mo1 O1 1.996(2) 3_657 y
Mo1 N3 2.113(3) . y
Mo1 N4 2.138(3) . y
Mo1 N2 2.180(3) . y
Mo1 N1 2.187(3) . y
Mo1 Mo1 2.3445(5) 3_657 y
Mo1 C1 2.608(3) . ?
Cl1 C31 1.712(11) . ?
Cl2A C31 1.598(10) . ?
Cl2B C31 1.55(3) . ?
O1 Mo1 1.996(2) 3_657 ?
O2 C5 1.362(4) . ?
O2 C8 1.436(5) . ?
O3 C12 1.383(4) . ?
O3 C15 1.412(5) . ?
O4 C20 1.368(4) . ?
O4 C23 1.413(6) . ?
O5 C27 1.374(4) . ?
O5 C30 1.423(5) . ?
N1 C1 1.319(4) . ?
N1 C2 1.414(4) . ?
N2 C1 1.324(4) . ?
N2 C9 1.420(4) . ?
N3 C16 1.332(4) . ?
N3 C17 1.435(4) . ?
N4 C16 1.319(4) 3_657 ?
N4 C24 1.447(4) . ?
C2 C7 1.389(5) . ?
C2 C3 1.402(4) . ?
C3 C4 1.384(5) . ?
C4 C5 1.386(5) . ?
C5 C6 1.401(5) . ?
C6 C7 1.383(5) . ?
C9 C14 1.386(5) . ?
C9 C10 1.389(5) . ?
C10 C11 1.379(5) . ?
C11 C12 1.366(5) . ?
C12 C13 1.380(6) . ?
C13 C14 1.377(6) . ?
C16 N4 1.319(4) 3_657 ?
C17 C22 1.363(5) . ?
C17 C18 1.381(5) . ?
C18 C19 1.390(5) . ?
C19 C20 1.386(6) . ?
C20 C21 1.367(6) . ?
C21 C22 1.384(6) . ?
C24 C25 1.374(5) . ?
C24 C29 1.394(5) . ?
C25 C26 1.403(4) . ?
C26 C27 1.390(5) . ?
C27 C28 1.376(5) . ?
C28 C29 1.384(4) . ?
