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#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/24/4062423.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_4062423
loop_
_publ_author_name
'Kerstin Most, Nadia C. Moesch-Zanetti, Denis Vidovic, Joerg Magull'
_publ_section_title
;
Syntheses and structures of two molybdenum(IV)complexes
 with the ancillary ligands 3,5-dimethylpyrazole and
 3,5-di-tert-butylpyrazole. Contrasting coordination modes and
 C-H activation in NMe2'
;
_journal_name_full               Organometallics
_journal_year                    2003
_chemical_formula_moiety         'C22 H35 Mo N9, 0.5(C6 H14)'
_chemical_formula_sum            'C25 H42 Mo N9'
_chemical_formula_weight         564.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                100.95(3)
_cell_angle_beta                 108.62(3)
_cell_angle_gamma                105.31(3)
_cell_formula_units_Z            2
_cell_length_a                   9.255(2)
_cell_length_b                   12.931(3)
_cell_length_c                   13.565(3)
_cell_measurement_temperature    133(2)
_cell_volume                     1415.4(6)
_diffrn_ambient_temperature      133(2)
_exptl_crystal_density_diffrn    1.325
_cod_database_code               4062423
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
Mo1 Mo 0.28454(4) 0.24845(3) 0.33730(3) 0.01924(12) Uani 1 1 d . . .
N1 N 0.5296(4) 0.2705(3) 0.3698(3) 0.0248(8) Uani 1 1 d . . .
N2 N 0.4468(4) 0.1574(3) 0.3451(3) 0.0238(7) Uani 1 1 d . . .
N3 N 0.3145(4) 0.2823(3) 0.5050(3) 0.0227(7) Uani 1 1 d . . .
N4 N 0.1823(4) 0.2984(3) 0.5249(3) 0.0257(8) Uani 1 1 d . . .
N5 N 0.0619(4) 0.1114(3) 0.2934(3) 0.0230(7) Uani 1 1 d . . .
N6 N -0.0751(4) 0.0955(3) 0.2031(3) 0.0260(8) Uani 1 1 d . . .
N7 N 0.2377(4) 0.2332(3) 0.1633(3) 0.0257(8) Uani 1 1 d . . .
N8 N 0.0855(5) 0.1697(3) 0.0868(3) 0.0263(8) Uani 1 1 d . . .
H8A H 0.005(7) 0.139(4) 0.114(4) 0.035(13) Uiso 1 1 d . . .
N9 N 0.1436(4) 0.3564(3) 0.3345(3) 0.0249(8) Uani 1 1 d . . .
H9 H 0.112(7) 0.355(4) 0.387(4) 0.039(15) Uiso 1 1 d . . .
C1 C 0.6876(5) 0.2867(4) 0.3936(3) 0.0257(9) Uani 1 1 d . . .
C2 C 0.7082(5) 0.1829(4) 0.3824(3) 0.0281(9) Uani 1 1 d . . .
H2A H 0.8067 0.1686 0.3924 0.034 Uiso 1 1 calc R . .
C3 C 0.5532(5) 0.1036(4) 0.3531(3) 0.0252(9) Uani 1 1 d . . .
C4 C 0.8098(5) 0.4018(4) 0.4288(4) 0.0360(11) Uani 1 1 d . . .
H4B H 0.7545 0.4568 0.4271 0.054 Uiso 1 1 calc R . .
H4C H 0.8670 0.4063 0.3793 0.054 Uiso 1 1 calc R . .
H4D H 0.8883 0.4179 0.5031 0.054 Uiso 1 1 calc R . .
C5 C 0.5012(6) -0.0203(4) 0.3334(4) 0.0324(10) Uani 1 1 d . . .
H5A H 0.3836 -0.0511 0.3137 0.049 Uiso 1 1 calc R . .
H5B H 0.5581 -0.0366 0.3998 0.049 Uiso 1 1 calc R . .
H5C H 0.5278 -0.0547 0.2738 0.049 Uiso 1 1 calc R . .
C6 C 0.4312(5) 0.2912(3) 0.6014(3) 0.0237(9) Uani 1 1 d . . .
C7 C 0.3746(6) 0.3125(4) 0.6830(4) 0.0291(10) Uani 1 1 d . . .
H7A H 0.4295 0.3226 0.7583 0.035 Uiso 1 1 calc R . .
C8 C 0.2194(6) 0.3160(4) 0.6316(3) 0.0278(9) Uani 1 1 d . . .
C9 C 0.5919(5) 0.2803(4) 0.6122(4) 0.0290(9) Uani 1 1 d . . .
H9A H 0.5979 0.2649 0.5403 0.043 Uiso 1 1 calc R . .
H9B H 0.6037 0.2184 0.6422 0.043 Uiso 1 1 calc R . .
H9C H 0.6795 0.3505 0.6612 0.043 Uiso 1 1 calc R . .
C10 C 0.0991(6) 0.3344(4) 0.6803(4) 0.0372(11) Uani 1 1 d . . .
H10A H 0.0008 0.3320 0.6229 0.056 Uiso 1 1 calc R . .
H10B H 0.1479 0.4078 0.7361 0.056 Uiso 1 1 calc R . .
H10C H 0.0707 0.2752 0.7136 0.056 Uiso 1 1 calc R . .
C11 C 0.0254(5) 0.0290(3) 0.3390(3) 0.0232(9) Uani 1 1 d . . .
C12 C -0.1347(5) -0.0410(4) 0.2789(3) 0.0261(9) Uani 1 1 d . . .
H12A H -0.1930 -0.1057 0.2920 0.031 Uiso 1 1 calc R . .
C13 C -0.1921(5) 0.0040(4) 0.1952(3) 0.0279(9) Uani 1 1 d . . .
C14 C 0.1452(5) 0.0185(4) 0.4373(4) 0.0282(9) Uani 1 1 d . . .
H14A H 0.2491 0.0803 0.4624 0.042 Uiso 1 1 calc R . .
H14B H 0.1616 -0.0534 0.4186 0.042 Uiso 1 1 calc R . .
H14C H 0.1037 0.0217 0.4954 0.042 Uiso 1 1 calc R . .
C15 C -0.3573(6) -0.0344(5) 0.1050(4) 0.0403(12) Uani 1 1 d . . .
H15A H -0.3577 0.0161 0.0595 0.061 Uiso 1 1 calc R . .
H15B H -0.4389 -0.0332 0.1364 0.061 Uiso 1 1 calc R . .
H15C H -0.3832 -0.1110 0.0603 0.061 Uiso 1 1 calc R . .
C16 C 0.3214(6) 0.2811(4) 0.1083(4) 0.0320(10) Uani 1 1 d . . .
C17 C 0.2203(6) 0.2474(4) -0.0017(4) 0.0349(11) Uani 1 1 d . . .
H17A H 0.2485 0.2685 -0.0583 0.042 Uiso 1 1 calc R . .
C18 C 0.0717(6) 0.1779(4) -0.0123(3) 0.0311(10) Uani 1 1 d . . .
C19 C 0.4957(6) 0.3564(5) 0.1621(4) 0.0442(13) Uani 1 1 d . . .
H19A H 0.5351 0.3653 0.2404 0.066 Uiso 1 1 calc R . .
H19B H 0.5056 0.4301 0.1505 0.066 Uiso 1 1 calc R . .
H19C H 0.5608 0.3233 0.1305 0.066 Uiso 1 1 calc R . .
C20 C -0.0871(6) 0.1165(4) -0.1091(4) 0.0393(11) Uani 1 1 d . . .
H20A H -0.1678 0.0743 -0.0855 0.059 Uiso 1 1 calc R . .
H20B H -0.0710 0.0643 -0.1637 0.059 Uiso 1 1 calc R . .
H20C H -0.1260 0.1708 -0.1409 0.059 Uiso 1 1 calc R . .
C21 C 0.3097(5) 0.4205(4) 0.3626(4) 0.0269(9) Uani 1 1 d . . .
H21A H 0.3708 0.4705 0.4385 0.032 Uiso 1 1 calc R . .
H21B H 0.3346 0.4548 0.3079 0.032 Uiso 1 1 calc R . .
C22 C 0.0155(6) 0.3629(4) 0.2407(4) 0.0322(10) Uani 1 1 d . . .
H22A H -0.0263 0.4206 0.2656 0.048 Uiso 1 1 calc R . .
H22B H -0.0732 0.2900 0.2063 0.048 Uiso 1 1 calc R . .
H22C H 0.0607 0.3825 0.1877 0.048 Uiso 1 1 calc R . .
C1L C -0.3124(16) 0.3129(9) -0.0478(11) 0.150(5) Uiso 1 1 d D . .
H1L1 H -0.3346 0.2806 -0.1249 0.225 Uiso 1 1 calc R . .
H1L2 H -0.4154 0.3032 -0.0385 0.225 Uiso 1 1 calc R . .
H1L3 H -0.2517 0.2745 -0.0040 0.225 Uiso 1 1 calc R . .
C2L C -0.2157(10) 0.4330(7) -0.0120(7) 0.083(2) Uiso 1 1 d D . .
H2LA H -0.1925 0.4664 0.0658 0.099 Uiso 1 1 calc R . .
H2LB H -0.2760 0.4727 -0.0554 0.099 Uiso 1 1 calc R . .
C3L C -0.0557(10) 0.4441(6) -0.0283(6) 0.076(2) Uiso 1 1 d . . .
H3LA H -0.0090 0.3900 0.0001 0.091 Uiso 1 1 calc R . .
H3LB H -0.0769 0.4271 -0.1070 0.091 Uiso 1 1 calc R . .
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 2.096(4) . ?
Mo1 C21 2.123(4) . ?
Mo1 N2 2.129(3) . ?
Mo1 N3 2.144(3) . ?
Mo1 N9 2.145(3) . ?
Mo1 N5 2.152(4) . ?
Mo1 N7 2.219(4) . ?
N1 C1 1.340(5) . ?
N1 N2 1.377(5) . ?
N2 C3 1.337(5) . ?
N3 C6 1.366(5) . ?
N3 N4 1.392(5) . ?
N4 C8 1.334(6) . ?
N5 C11 1.351(5) . ?
N5 N6 1.388(5) . ?
N6 C13 1.336(6) . ?
N7 C16 1.353(6) . ?
N7 N8 1.367(5) . ?
N8 C18 1.336(6) . ?
N8 H8A 0.96(5) . ?
N9 C21 1.424(6) . ?
N9 C22 1.470(5) . ?
N9 H9 0.85(5) . ?
C1 C2 1.392(6) . ?
C1 C4 1.489(6) . ?
C2 C3 1.404(6) . ?
C2 H2A 0.9500 . ?
C3 C5 1.489(6) . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.380(6) . ?
C6 C9 1.494(6) . ?
C7 C8 1.400(6) . ?
C7 H7A 0.9500 . ?
C8 C10 1.510(6) . ?
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 1.385(6) . ?
C11 C14 1.494(6) . ?
C12 C13 1.393(6) . ?
C12 H12A 0.9500 . ?
C13 C15 1.502(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.391(7) . ?
C16 C19 1.494(7) . ?
C17 C18 1.376(7) . ?
C17 H17A 0.9500 . ?
C18 C20 1.506(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C1L C2L 1.466(8) . ?
C1L H1L1 0.9800 . ?
C1L H1L2 0.9800 . ?
C1L H1L3 0.9800 . ?
C2L C3L 1.540(11) . ?
C2L H2LA 0.9900 . ?
C2L H2LB 0.9900 . ?
C3L C3L 1.425(15) 2_565 ?
C3L H3LA 0.9900 . ?
C3L H3LB 0.9900 . ?
