#------------------------------------------------------------------------------
#$Date: 2019-11-24 10:21:44 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237616 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/85/4088502.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_4088502
loop_
_publ_author_name
'Harisomayajula, N. V. Satyachand'
'Chen, Han-Gung'
'Kuo, Ting-Shen'
'Tsai, Yi-Chou'
_publ_section_title
;
 Reductive Cleavage of Acyl Halides to Carboxylato Alkylidyne Complexes
 from Their Reactions with the Quintuply Bonded Dimolybdenum Amidinate
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1534
_journal_paper_doi               10.1021/acs.organomet.6b00132
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C132 H166 F4 Mo4 N8 O5'
_chemical_formula_sum            'C132 H166 F4 Mo4 N8 O5'
_chemical_formula_weight         2404.49
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                99.5940(10)
_cell_angle_beta                 92.2550(10)
_cell_angle_gamma                107.6240(10)
_cell_formula_units_Z            1
_cell_length_a                   11.4489(8)
_cell_length_b                   13.0431(8)
_cell_length_c                   21.9598(15)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.72
_cell_volume                     3067.5(4)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX2'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25071
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.8590
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.726
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         10627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0347
_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)+(0.0821P)²+0.3640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                8880
_reflns_number_total             10627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00132_si_003.cif
_cod_data_source_block           compound_23
_cod_database_code               4088502
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
C1 C 0.6360(3) 0.0345(3) 0.34123(16) 0.0260(7) Uani 1 1 d . . .
C2 C 0.5996(3) -0.0803(3) 0.32755(18) 0.0362(9) Uani 1 1 d . . .
C3 C 0.6436(4) -0.1414(3) 0.2738(2) 0.0514(12) Uani 1 1 d . . .
H3 H 0.7199 -0.0899 0.2621 0.062 Uiso 1 1 calc R . .
C4 C 0.5443(6) -0.1743(4) 0.2180(2) 0.089(2) Uani 1 1 d . . .
H4A H 0.5712 -0.2146 0.1825 0.134 Uiso 1 1 calc R . .
H4B H 0.5321 -0.1082 0.2070 0.134 Uiso 1 1 calc R . .
H4C H 0.4666 -0.2209 0.2292 0.134 Uiso 1 1 calc R . .
C5 C 0.6754(4) -0.2418(3) 0.2881(3) 0.0617(13) Uani 1 1 d . . .
H5A H 0.7030 -0.2776 0.2511 0.093 Uiso 1 1 calc R . .
H5B H 0.6022 -0.2934 0.3002 0.093 Uiso 1 1 calc R . .
H5C H 0.7412 -0.2184 0.3222 0.093 Uiso 1 1 calc R . .
C6 C 0.5143(4) -0.1386(3) 0.3638(2) 0.0498(11) Uani 1 1 d . . .
H6 H 0.4913 -0.2162 0.3564 0.060 Uiso 1 1 calc R . .
C7 C 0.4642(4) -0.0859(4) 0.4091(2) 0.0565(13) Uani 1 1 d . . .
H7 H 0.4045 -0.1269 0.4321 0.068 Uiso 1 1 calc R . .
C8 C 0.5001(4) 0.0273(3) 0.42189(19) 0.0465(11) Uani 1 1 d . . .
H8 H 0.4650 0.0630 0.4541 0.056 Uiso 1 1 calc R . .
C9 C 0.5864(3) 0.0903(3) 0.38872(17) 0.0324(8) Uani 1 1 d . . .
C10 C 0.6252(4) 0.2140(3) 0.40496(18) 0.0387(9) Uani 1 1 d . . .
H10 H 0.6425 0.2425 0.3656 0.046 Uiso 1 1 calc R . .
C11 C 0.7432(5) 0.2575(4) 0.4477(3) 0.0782(17) Uani 1 1 d . . .
H11A H 0.7682 0.3377 0.4572 0.117 Uiso 1 1 calc R . .
H11B H 0.8081 0.2343 0.4273 0.117 Uiso 1 1 calc R . .
H11C H 0.7300 0.2287 0.4862 0.117 Uiso 1 1 calc R . .
C12 C 0.5286(4) 0.2594(4) 0.4338(2) 0.0630(13) Uani 1 1 d . . .
H12A H 0.5601 0.3396 0.4423 0.095 Uiso 1 1 calc R . .
H12B H 0.5098 0.2331 0.4727 0.095 Uiso 1 1 calc R . .
H12C H 0.4537 0.2348 0.4051 0.095 Uiso 1 1 calc R . .
C13 C 0.6955(3) 0.1471(3) 0.26502(15) 0.0231(7) Uani 1 1 d . . .
H13 H 0.6113 0.1421 0.2586 0.028 Uiso 1 1 calc R . .
C14 C 0.7334(3) 0.2632(3) 0.19065(16) 0.0264(7) Uani 1 1 d . . .
C15 C 0.7112(3) 0.2191(3) 0.12698(17) 0.0346(8) Uani 1 1 d . . .
C16 C 0.7174(4) 0.1054(3) 0.10142(18) 0.0411(9) Uani 1 1 d . . .
H16 H 0.7693 0.0861 0.1326 0.049 Uiso 1 1 calc R . .
C17 C 0.5881(5) 0.0212(4) 0.0943(2) 0.0665(14) Uani 1 1 d . . .
H17A H 0.5929 -0.0519 0.0780 0.100 Uiso 1 1 calc R . .
H17B H 0.5339 0.0402 0.0654 0.100 Uiso 1 1 calc R . .
H17C H 0.5551 0.0218 0.1348 0.100 Uiso 1 1 calc R . .
C18 C 0.7760(5) 0.0984(4) 0.0402(2) 0.0594(13) Uani 1 1 d . . .
H18A H 0.7787 0.0237 0.0266 0.089 Uiso 1 1 calc R . .
H18B H 0.8599 0.1498 0.0462 0.089 Uiso 1 1 calc R . .
H18C H 0.7272 0.1171 0.0087 0.089 Uiso 1 1 calc R . .
C19 C 0.6791(4) 0.2804(4) 0.08708(19) 0.0480(11) Uani 1 1 d . . .
H19 H 0.6624 0.2513 0.0439 0.058 Uiso 1 1 calc R . .
C20 C 0.6712(4) 0.3822(4) 0.1094(2) 0.0570(13) Uani 1 1 d . . .
H20 H 0.6511 0.4239 0.0814 0.068 Uiso 1 1 calc R . .
C21 C 0.6920(4) 0.4245(3) 0.1715(2) 0.0459(10) Uani 1 1 d . . .
H21 H 0.6846 0.4949 0.1861 0.055 Uiso 1 1 calc R . .
C22 C 0.7236(3) 0.3670(3) 0.21394(18) 0.0331(8) Uani 1 1 d . . .
C23 C 0.7425(3) 0.4159(3) 0.28261(18) 0.0373(9) Uani 1 1 d . . .
H23 H 0.7762 0.3684 0.3047 0.045 Uiso 1 1 calc R . .
C24 C 0.6195(4) 0.4161(4) 0.3076(2) 0.0505(11) Uani 1 1 d . . .
H24A H 0.6333 0.4472 0.3521 0.076 Uiso 1 1 calc R . .
H24B H 0.5634 0.3408 0.3010 0.076 Uiso 1 1 calc R . .
H24C H 0.5830 0.4603 0.2857 0.076 Uiso 1 1 calc R . .
C25 C 0.8341(4) 0.5315(3) 0.2973(2) 0.0577(13) Uani 1 1 d . . .
H25A H 0.8434 0.5590 0.3422 0.087 Uiso 1 1 calc R . .
H25B H 0.8037 0.5798 0.2758 0.087 Uiso 1 1 calc R . .
H25C H 0.9140 0.5300 0.2835 0.087 Uiso 1 1 calc R . .
C26 C 1.2503(3) 0.3434(3) 0.25903(16) 0.0249(7) Uani 1 1 d . . .
C27 C 1.2934(3) 0.3131(3) 0.20224(17) 0.0317(8) Uani 1 1 d . . .
C28 C 1.2633(3) 0.1940(3) 0.17100(18) 0.0395(9) Uani 1 1 d . . .
H28 H 1.1845 0.1520 0.1856 0.047 Uiso 1 1 calc R . .
C29 C 1.2453(5) 0.1762(4) 0.1001(2) 0.0669(15) Uani 1 1 d . . .
H29A H 1.2257 0.0980 0.0828 0.100 Uiso 1 1 calc R . .
H29B H 1.3211 0.2172 0.0845 0.100 Uiso 1 1 calc R . .
H29C H 1.1775 0.2019 0.0877 0.100 Uiso 1 1 calc R . .
C30 C 1.3635(4) 0.1494(4) 0.1919(3) 0.0650(14) Uani 1 1 d . . .
H30A H 1.3444 0.0726 0.1718 0.097 Uiso 1 1 calc R . .
H30B H 1.3676 0.1549 0.2371 0.097 Uiso 1 1 calc R . .
H30C H 1.4430 0.1922 0.1804 0.097 Uiso 1 1 calc R . .
C31 C 1.3710(3) 0.3958(3) 0.17582(19) 0.0415(10) Uani 1 1 d . . .
H31 H 1.4020 0.3771 0.1375 0.050 Uiso 1 1 calc R . .
C32 C 1.4030(4) 0.5035(3) 0.2045(2) 0.0453(10) Uani 1 1 d . . .
H32 H 1.4535 0.5587 0.1851 0.054 Uiso 1 1 calc R . .
C33 C 1.3624(3) 0.5322(3) 0.26120(19) 0.0399(9) Uani 1 1 d . . .
H33 H 1.3864 0.6071 0.2808 0.048 Uiso 1 1 calc R . .
C34 C 1.2869(3) 0.4532(3) 0.29027(17) 0.0314(8) Uani 1 1 d . . .
C35 C 1.2509(4) 0.4884(3) 0.35411(18) 0.0378(9) Uani 1 1 d . . .
H35 H 1.1891 0.4233 0.3652 0.045 Uiso 1 1 calc R . .
C36 C 1.1924(4) 0.5799(3) 0.3579(2) 0.0514(11) Uani 1 1 d . . .
H36A H 1.1712 0.5982 0.4003 0.077 Uiso 1 1 calc R . .
H36B H 1.1177 0.5554 0.3290 0.077 Uiso 1 1 calc R . .
H36C H 1.2509 0.6447 0.3469 0.077 Uiso 1 1 calc R . .
C37 C 1.3638(4) 0.5228(4) 0.4019(2) 0.0559(12) Uani 1 1 d . . .
H37A H 1.3401 0.5453 0.4432 0.084 Uiso 1 1 calc R . .
H37B H 1.4279 0.5842 0.3910 0.084 Uiso 1 1 calc R . .
H37C H 1.3954 0.4609 0.4021 0.084 Uiso 1 1 calc R . .
C38 C 1.1870(3) 0.2215(3) 0.33019(16) 0.0261(7) Uani 1 1 d . . .
H38 H 1.2710 0.2425 0.3460 0.031 Uiso 1 1 calc R . .
C39 C 1.1431(3) 0.1107(3) 0.40839(17) 0.0310(8) Uani 1 1 d . . .
C40 C 1.1799(3) 0.1786(3) 0.46709(18) 0.0366(9) Uani 1 1 d . . .
C41 C 1.1824(4) 0.2975(3) 0.47917(19) 0.0500(11) Uani 1 1 d . . .
H41 H 1.2000 0.3256 0.4397 0.060 Uiso 1 1 calc R . .
C42 C 1.0585(6) 0.3055(6) 0.4947(4) 0.132(3) Uani 1 1 d . . .
H42A H 0.9956 0.2591 0.4616 0.197 Uiso 1 1 calc R . .
H42B H 1.0595 0.3817 0.4985 0.197 Uiso 1 1 calc R . .
H42C H 1.0396 0.2808 0.5340 0.197 Uiso 1 1 calc R . .
C43 C 1.2804(5) 0.3712(4) 0.5289(2) 0.0737(16) Uani 1 1 d . . .
H43A H 1.3611 0.3661 0.5185 0.111 Uiso 1 1 calc R . .
H43B H 1.2631 0.3485 0.5689 0.111 Uiso 1 1 calc R . .
H43C H 1.2805 0.4471 0.5318 0.111 Uiso 1 1 calc R . .
C44 C 1.2122(4) 0.1326(4) 0.5155(2) 0.0503(11) Uani 1 1 d . . .
H44 H 1.2382 0.1772 0.5555 0.060 Uiso 1 1 calc R . .
C45 C 1.2074(4) 0.0254(4) 0.5069(2) 0.0586(13) Uani 1 1 d . . .
H45 H 1.2290 -0.0039 0.5409 0.070 Uiso 1 1 calc R . .
C46 C 1.1715(5) -0.0403(4) 0.4493(2) 0.0597(13) Uani 1 1 d . . .
H46 H 1.1684 -0.1149 0.4438 0.072 Uiso 1 1 calc R . .
C47 C 1.1397(4) 0.0010(3) 0.3990(2) 0.0429(10) Uani 1 1 d . . .
C48 C 1.1054(5) -0.0716(3) 0.3351(2) 0.0634(15) Uani 1 1 d . . .
H48 H 1.0403 -0.0496 0.3139 0.076 Uiso 1 1 calc R . .
C49 C 1.2134(7) -0.0499(5) 0.2971(3) 0.092(2) Uani 1 1 d . . .
H49A H 1.1894 -0.0963 0.2558 0.139 Uiso 1 1 calc R . .
H49B H 1.2813 -0.0665 0.3175 0.139 Uiso 1 1 calc R . .
H49C H 1.2399 0.0273 0.2930 0.139 Uiso 1 1 calc R . .
C50 C 1.0519(6) -0.1934(4) 0.3351(3) 0.096(2) Uani 1 1 d . . .
H50A H 0.9815 -0.2061 0.3600 0.144 Uiso 1 1 calc R . .
H50B H 1.1150 -0.2195 0.3529 0.144 Uiso 1 1 calc R . .
H50C H 1.0248 -0.2331 0.2924 0.144 Uiso 1 1 calc R . .
C51 C 0.9398(3) 0.0570(3) 0.23036(16) 0.0255(7) Uani 1 1 d . . .
C52 C 0.9382(3) -0.0358(3) 0.18234(17) 0.0305(8) Uani 1 1 d . . .
C53 C 0.9128(3) -0.1426(3) 0.19410(19) 0.0368(9) Uani 1 1 d . . .
H53 H 0.8960 -0.1558 0.2346 0.044 Uiso 1 1 calc R . .
C54 C 0.9117(4) -0.2289(3) 0.1479(2) 0.0523(12) Uani 1 1 d . . .
H54 H 0.8943 -0.3008 0.1563 0.063 Uiso 1 1 calc R . .
C55 C 0.9361(4) -0.2087(4) 0.0899(2) 0.0561(12) Uani 1 1 d . . .
C56 C 0.9618(4) -0.1066(4) 0.0760(2) 0.0550(12) Uani 1 1 d . . .
H56 H 0.9789 -0.0951 0.0353 0.066 Uiso 1 1 calc R . .
C57 C 0.9626(3) -0.0198(3) 0.12233(18) 0.0383(9) Uani 1 1 d . . .
H57 H 0.9800 0.0516 0.1130 0.046 Uiso 1 1 calc R . .
C58 C 1.0275(3) 0.3702(3) 0.18094(16) 0.0284(8) Uani 1 1 d . . .
C59 C 1.0762(3) 0.4658(3) 0.14959(18) 0.0331(8) Uani 1 1 d . . .
C60 C 1.0896(5) 0.4479(4) 0.0871(2) 0.0562(13) Uani 1 1 d . . .
H60 H 1.0646 0.3752 0.0640 0.067 Uiso 1 1 calc R . .
C61 C 1.1391(6) 0.5352(4) 0.0571(2) 0.0768(17) Uani 1 1 d . . .
H61 H 1.1463 0.5236 0.0137 0.092 Uiso 1 1 calc R . .
C62 C 1.1770(5) 0.6377(4) 0.0923(2) 0.0656(15) Uani 1 1 d . . .
C63 C 1.1637(4) 0.6598(3) 0.1531(2) 0.0549(12) Uani 1 1 d . . .
H63 H 1.1887 0.7331 0.1754 0.066 Uiso 1 1 calc R . .
C64 C 1.1125(4) 0.5724(3) 0.1825(2) 0.0448(10) Uani 1 1 d . . .
H64 H 1.1022 0.5858 0.2255 0.054 Uiso 1 1 calc R . .
C65 C 0.6006(15) 0.5952(12) 0.0063(8) 0.119(5) Uiso 0.50 1 d P A 1
H65A H 0.6752 0.5783 0.0197 0.143 Uiso 0.50 1 calc PR A 1
H65B H 0.6119 0.6153 -0.0351 0.143 Uiso 0.50 1 calc PR A 1
C65' C 0.5012(14) 0.5893(12) 0.0423(7) 0.111(5) Uiso 0.50 1 d P A 2
H65C H 0.4232 0.6046 0.0338 0.133 Uiso 0.50 1 calc PR A 2
H65D H 0.4994 0.5683 0.0836 0.133 Uiso 0.50 1 calc PR A 2
C66 C 0.5934(9) 0.6842(7) 0.0468(4) 0.150(3) Uiso 1 1 d . . .
H66A H 0.6679 0.7462 0.0473 0.225 Uiso 1 1 calc R A 1
H66B H 0.5859 0.6669 0.0885 0.225 Uiso 1 1 calc R A 1
H66C H 0.5211 0.7034 0.0336 0.225 Uiso 1 1 calc R A 1
N1 N 0.7301(2) 0.0957(2) 0.30702(12) 0.0228(6) Uani 1 1 d . . .
N2 N 0.7756(2) 0.2043(2) 0.23250(12) 0.0226(6) Uani 1 1 d . . .
N3 N 1.1571(2) 0.2619(2) 0.28282(13) 0.0238(6) Uani 1 1 d . . .
N4 N 1.1023(3) 0.1519(2) 0.35660(13) 0.0260(6) Uani 1 1 d . . .
O1 O 1.0095(2) 0.27500(18) 0.15283(11) 0.0330(6) Uani 1 1 d . . .
O2 O 1.0091(2) 0.38922(18) 0.23864(11) 0.0296(5) Uani 1 1 d . . .
O3 O 0.5000 0.5000 0.0000 0.128(3) Uiso 1 2 d S . .
Mo1 Mo 0.91827(2) 0.10979(2) 0.317842(13) 0.02113(10) Uani 1 1 d . . .
Mo2 Mo 0.96579(2) 0.21688(2) 0.249273(13) 0.02098(10) Uani 1 1 d . . .
F1 F 0.9341(3) -0.2936(2) 0.04448(14) 0.0925(11) Uani 1 1 d . . .
F2 F 1.2280(4) 0.7243(2) 0.06392(17) 0.1070(13) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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
C2 C1 C9 121.3(3) . .
C2 C1 N1 118.7(3) . .
C9 C1 N1 120.0(3) . .
C1 C2 C6 118.1(3) . .
C1 C2 C3 122.0(3) . .
C6 C2 C3 119.8(3) . .
C2 C3 C5 114.0(4) . .
C2 C3 C4 108.3(4) . .
C5 C3 C4 111.1(4) . .
C2 C3 H3 107.8 . .
C5 C3 H3 107.8 . .
C4 C3 H3 107.8 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 C2 121.3(4) . .
C7 C6 H6 119.3 . .
C2 C6 H6 119.3 . .
C6 C7 C8 120.0(4) . .
C6 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
C7 C8 C9 121.7(4) . .
C7 C8 H8 119.2 . .
C9 C8 H8 119.2 . .
C8 C9 C1 117.6(3) . .
C8 C9 C10 120.1(3) . .
C1 C9 C10 122.3(3) . .
C9 C10 C11 110.3(3) . .
C9 C10 C12 114.4(3) . .
C11 C10 C12 109.4(4) . .
C9 C10 H10 107.5 . .
C11 C10 H10 107.5 . .
C12 C10 H10 107.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N2 C13 N1 121.4(3) . .
N2 C13 H13 119.3 . .
N1 C13 H13 119.3 . .
C15 C14 C22 121.1(3) . .
C15 C14 N2 119.4(3) . .
C22 C14 N2 119.3(3) . .
C19 C15 C14 118.5(3) . .
C19 C15 C16 119.8(3) . .
C14 C15 C16 121.6(3) . .
C15 C16 C18 113.3(3) . .
C15 C16 C17 110.0(3) . .
C18 C16 C17 110.5(4) . .
C15 C16 H16 107.6 . .
C18 C16 H16 107.6 . .
C17 C16 H16 107.6 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 C15 120.7(4) . .
C20 C19 H19 119.7 . .
C15 C19 H19 119.7 . .
C21 C20 C19 120.6(4) . .
C21 C20 H20 119.7 . .
C19 C20 H20 119.7 . .
C20 C21 C22 121.5(4) . .
C20 C21 H21 119.2 . .
C22 C21 H21 119.2 . .
C21 C22 C14 117.6(4) . .
C21 C22 C23 119.6(3) . .
C14 C22 C23 122.8(3) . .
C22 C23 C25 112.8(3) . .
C22 C23 C24 110.6(3) . .
C25 C23 C24 109.9(3) . .
C22 C23 H23 107.8 . .
C25 C23 H23 107.8 . .
C24 C23 H23 107.8 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C23 C25 H25A 109.5 . .
C23 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C23 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C27 C26 C34 121.4(3) . .
C27 C26 N3 119.0(3) . .
C34 C26 N3 119.3(3) . .
C26 C27 C31 118.1(3) . .
C26 C27 C28 121.8(3) . .
C31 C27 C28 120.0(3) . .
C27 C28 C30 109.3(3) . .
C27 C28 C29 113.4(4) . .
C30 C28 C29 110.9(4) . .
C27 C28 H28 107.7 . .
C30 C28 H28 107.7 . .
C29 C28 H28 107.7 . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C28 C30 H30A 109.5 . .
C28 C30 H30B 109.5 . .
H30A C30 H30B 109.5 . .
C28 C30 H30C 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C32 C31 C27 121.0(4) . .
C32 C31 H31 119.5 . .
C27 C31 H31 119.5 . .
C31 C32 C33 120.5(3) . .
C31 C32 H32 119.8 . .
C33 C32 H32 119.8 . .
C32 C33 C34 121.1(3) . .
C32 C33 H33 119.5 . .
C34 C33 H33 119.5 . .
C33 C34 C26 117.8(3) . .
C33 C34 C35 118.9(3) . .
C26 C34 C35 123.2(3) . .
C34 C35 C36 113.9(3) . .
C34 C35 C37 109.7(3) . .
C36 C35 C37 110.2(3) . .
C34 C35 H35 107.6 . .
C36 C35 H35 107.6 . .
C37 C35 H35 107.6 . .
C35 C36 H36A 109.5 . .
C35 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C35 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
C35 C37 H37A 109.5 . .
C35 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C35 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
N3 C38 N4 121.8(3) . .
N3 C38 H38 119.1 . .
N4 C38 H38 119.1 . .
C47 C39 C40 121.0(3) . .
C47 C39 N4 118.4(3) . .
C40 C39 N4 120.5(3) . .
C44 C40 C39 117.6(4) . .
C44 C40 C41 120.0(4) . .
C39 C40 C41 122.4(3) . .
C42 C41 C43 109.8(5) . .
C42 C41 C40 110.4(4) . .
C43 C41 C40 114.2(4) . .
C42 C41 H41 107.3 . .
C43 C41 H41 107.3 . .
C40 C41 H41 107.3 . .
C41 C42 H42A 109.5 . .
C41 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
C41 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C41 C43 H43A 109.5 . .
C41 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C41 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C45 C44 C40 121.7(4) . .
C45 C44 H44 119.1 . .
C40 C44 H44 119.1 . .
C44 C45 C46 120.2(4) . .
C44 C45 H45 119.9 . .
C46 C45 H45 119.9 . .
C45 C46 C47 120.8(4) . .
C45 C46 H46 119.6 . .
C47 C46 H46 119.6 . .
C46 C47 C39 118.6(4) . .
C46 C47 C48 120.0(4) . .
C39 C47 C48 121.4(3) . .
C49 C48 C47 110.4(4) . .
C49 C48 C50 110.6(5) . .
C47 C48 C50 115.0(4) . .
C49 C48 H48 106.8 . .
C47 C48 H48 106.8 . .
C50 C48 H48 106.8 . .
C48 C49 H49A 109.5 . .
C48 C49 H49B 109.5 . .
H49A C49 H49B 109.5 . .
C48 C49 H49C 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
C48 C50 H50A 109.5 . .
C48 C50 H50B 109.5 . .
H50A C50 H50B 109.5 . .
C48 C50 H50C 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C52 C51 Mo1 147.4(3) . .
C52 C51 Mo2 145.3(3) . .
Mo1 C51 Mo2 67.25(10) . .
C57 C52 C53 117.7(3) . .
C57 C52 C51 119.9(3) . .
C53 C52 C51 122.4(3) . .
C54 C53 C52 121.3(4) . .
C54 C53 H53 119.4 . .
C52 C53 H53 119.4 . .
C55 C54 C53 118.7(4) . .
C55 C54 H54 120.6 . .
C53 C54 H54 120.6 . .
F1 C55 C56 118.9(4) . .
F1 C55 C54 118.7(4) . .
C56 C55 C54 122.4(4) . .
C55 C56 C57 119.0(4) . .
C55 C56 H56 120.5 . .
C57 C56 H56 120.5 . .
C56 C57 C52 120.9(4) . .
C56 C57 H57 119.5 . .
C52 C57 H57 119.5 . .
O1 C58 O2 120.7(3) . .
O1 C58 C59 121.0(3) . .
O2 C58 C59 118.3(3) . .
C60 C59 C64 119.0(4) . .
C60 C59 C58 119.6(3) . .
C64 C59 C58 121.4(4) . .
C59 C60 C61 120.8(4) . .
C59 C60 H60 119.6 . .
C61 C60 H60 119.6 . .
C62 C61 C60 117.5(5) . .
C62 C61 H61 121.3 . .
C60 C61 H61 121.3 . .
C63 C62 C61 124.0(4) . .
C63 C62 F2 117.6(4) . .
C61 C62 F2 118.4(5) . .
C62 C63 C64 118.1(4) . .
C62 C63 H63 120.9 . .
C64 C63 H63 120.9 . .
C59 C64 C63 120.5(4) . .
C59 C64 H64 119.8 . .
C63 C64 H64 119.8 . .
C66 C65 O3 116.2(12) . .
C66 C65 H65A 108.2 . .
O3 C65 H65A 108.2 . .
C66 C65 H65B 108.2 . .
O3 C65 H65B 108.2 . .
H65A C65 H65B 107.4 . .
C66 C65' O3 120.2(12) . .
C66 C65' H65C 107.3 . .
O3 C65' H65C 107.3 . .
C66 C65' H65D 107.3 . .
O3 C65' H65D 107.3 . .
H65C C65' H65D 106.9 . .
C65' C66 C65 62.2(9) . .
C65' C66 H66A 171.2 . .
C65 C66 H66A 109.5 . .
C65' C66 H66B 72.4 . .
C65 C66 H66B 109.5 . .
H66A C66 H66B 109.5 . .
C65' C66 H66C 77.3 . .
C65 C66 H66C 109.5 . .
H66A C66 H66C 109.5 . .
H66B C66 H66C 109.5 . .
C13 N1 C1 118.0(3) . .
C13 N1 Mo1 117.0(2) . .
C1 N1 Mo1 125.0(2) . .
C13 N2 C14 118.5(3) . .
C13 N2 Mo2 118.4(2) . .
C14 N2 Mo2 122.9(2) . .
C38 N3 C26 119.7(3) . .
C38 N3 Mo2 118.6(2) . .
C26 N3 Mo2 121.4(2) . .
C38 N4 C39 118.3(3) . .
C38 N4 Mo1 116.2(2) . .
C39 N4 Mo1 125.5(2) . .
C58 O1 Mo2 87.4(2) . .
C58 O2 Mo2 94.6(2) . .
C65' O3 C65' 180.0(15) . 2_665
C65' O3 C65 61.1(9) . .
C65' O3 C65 118.9(9) 2_665 .
C65' O3 C65 118.9(9) . 2_665
C65' O3 C65 61.1(9) 2_665 2_665
C65 O3 C65 180.0(14) . 2_665
C51 Mo1 N1 98.69(12) . .
C51 Mo1 N4 99.21(12) . .
N1 Mo1 N4 161.71(11) . .
C51 Mo1 Mo2 56.43(9) . .
N1 Mo1 Mo2 93.02(7) . .
N4 Mo1 Mo2 93.75(7) . .
C51 Mo2 N2 95.74(11) . .
C51 Mo2 N3 95.46(11) . .
N2 Mo2 N3 166.38(10) . .
C51 Mo2 Mo1 56.32(10) . .
N2 Mo2 Mo1 90.14(7) . .
N3 Mo2 Mo1 89.64(7) . .
C51 Mo2 O2 161.27(11) . .
N2 Mo2 O2 86.81(9) . .
N3 Mo2 O2 85.07(9) . .
Mo1 Mo2 O2 142.37(6) . .
C51 Mo2 O1 104.25(11) . .
N2 Mo2 O1 91.07(9) . .
N3 Mo2 O1 93.65(9) . .
Mo1 Mo2 O1 160.54(6) . .
O2 Mo2 O1 57.08(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.403(5) .
C1 C9 1.410(5) .
C1 N1 1.450(4) .
C2 C6 1.406(5) .
C2 C3 1.503(5) .
C3 C5 1.537(6) .
C3 C4 1.549(7) .
C3 H3 1.0000 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.360(6) .
C6 H6 0.9500 .
C7 C8 1.383(6) .
C7 H7 0.9500 .
C8 C9 1.395(5) .
C8 H8 0.9500 .
C9 C10 1.513(5) .
C10 C11 1.512(6) .
C10 C12 1.516(5) .
C10 H10 1.0000 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 N2 1.312(4) .
C13 N1 1.340(4) .
C13 H13 0.9500 .
C14 C15 1.402(5) .
C14 C22 1.404(5) .
C14 N2 1.447(4) .
C15 C19 1.388(5) .
C15 C16 1.520(5) .
C16 C18 1.527(5) .
C16 C17 1.536(6) .
C16 H16 1.0000 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 C20 1.368(6) .
C19 H19 0.9500 .
C20 C21 1.367(6) .
C20 H20 0.9500 .
C21 C22 1.390(5) .
C21 H21 0.9500 .
C22 C23 1.516(5) .
C23 C25 1.527(5) .
C23 C24 1.532(5) .
C23 H23 1.0000 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 C27 1.398(5) .
C26 C34 1.409(5) .
C26 N3 1.443(4) .
C27 C31 1.400(5) .
C27 C28 1.518(5) .
C28 C30 1.522(6) .
C28 C29 1.532(6) .
C28 H28 1.0000 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 C32 1.370(5) .
C31 H31 0.9500 .
C32 C33 1.380(6) .
C32 H32 0.9500 .
C33 C34 1.393(5) .
C33 H33 0.9500 .
C34 C35 1.514(5) .
C35 C36 1.528(5) .
C35 C37 1.536(6) .
C35 H35 1.0000 .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C38 N3 1.319(4) .
C38 N4 1.337(4) .
C38 H38 0.9500 .
C39 C47 1.399(5) .
C39 C40 1.405(5) .
C39 N4 1.454(4) .
C40 C44 1.393(5) .
C40 C41 1.520(5) .
C41 C42 1.502(7) .
C41 C43 1.509(6) .
C41 H41 1.0000 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 C45 1.363(6) .
C44 H44 0.9500 .
C45 C46 1.375(7) .
C45 H45 0.9500 .
C46 C47 1.389(6) .
C46 H46 0.9500 .
C47 C48 1.519(6) .
C48 C49 1.502(8) .
C48 C50 1.519(6) .
C48 H48 1.0000 .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
C51 C52 1.462(5) .
C51 Mo1 1.981(3) .
C51 Mo2 1.984(3) .
C52 C57 1.394(5) .
C52 C53 1.405(5) .
C53 C54 1.379(5) .
C53 H53 0.9500 .
C54 C55 1.366(6) .
C54 H54 0.9500 .
C55 F1 1.355(5) .
C55 C56 1.364(6) .
C56 C57 1.388(6) .
C56 H56 0.9500 .
C57 H57 0.9500 .
C58 O1 1.243(4) .
C58 O2 1.288(4) .
C58 C59 1.495(5) .
C59 C60 1.377(6) .
C59 C64 1.386(5) .
C60 C61 1.393(6) .
C60 H60 0.9500 .
C61 C62 1.360(7) .
C61 H61 0.9500 .
C62 C63 1.344(7) .
C62 F2 1.366(5) .
C63 C64 1.390(5) .
C63 H63 0.9500 .
C64 H64 0.9500 .
C65 C66 1.366(16) .
C65 O3 1.397(15) .
C65 H65A 0.9900 .
C65 H65B 0.9900 .
C65' C66 1.348(14) .
C65' O3 1.359(15) .
C65' H65C 0.9900 .
C65' H65D 0.9900 .
C66 H66A 0.9800 .
C66 H66B 0.9800 .
C66 H66C 0.9800 .
N1 Mo1 2.107(3) .
N2 Mo2 2.145(3) .
N3 Mo2 2.153(3) .
N4 Mo1 2.114(3) .
O1 Mo2 2.387(2) .
O2 Mo2 2.205(2) .
O3 C65' 1.359(15) 2_665
O3 C65 1.397(15) 2_665
Mo1 Mo2 2.1954(4) .
