#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179247 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/67/4316795.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_4316795
loop_
_publ_author_name
'Victor W. L. Ng'
'Michelle K. Taylor'
'Jonathan M. White'
'Charles G. Young'
_publ_section_title
;
 cis-Dioxo- and cis-(Hydroxo)oxo-Mo(V) Complexes Stabilized by
 Intramolecular Hydrogen-Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9460
_journal_page_last               9469
_journal_paper_doi               10.1021/ic1011428
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C32 H40 B Mo N7 O4'
_chemical_formula_weight         693.46
_chemical_name_common            Tp(iPr)MoO2(OAr-2-CON(Me)Ph)
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                92.468(6)
_cell_angle_beta                 97.569(7)
_cell_angle_gamma                103.852(8)
_cell_formula_units_Z            2
_cell_length_a                   8.7355(8)
_cell_length_b                   11.2816(9)
_cell_length_c                   17.2653(12)
_cell_measurement_reflns_used    7185
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.1679
_cell_measurement_theta_min      4.9526
_cell_volume                     1632.7(2)
_computing_cell_refinement
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10520
_diffrn_reflns_theta_full        74.05
_diffrn_reflns_theta_max         74.05
_diffrn_reflns_theta_min         4.97
_exptl_absorpt_coefficient_mu    3.671
_exptl_absorpt_correction_T_max  0.7831
_exptl_absorpt_correction_T_min  0.3862
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;    
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.3249
_exptl_crystal_size_mid          0.1024
_exptl_crystal_size_min          0.0660
_refine_diff_density_max         1.307
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0466
_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)+(0.0921P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                5507
_reflns_number_total             6243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011428_si_002_4.cif
_cod_data_source_block           jmwng20
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4316795
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 0.1814(4) 0.2983(3) 0.14540(19) 0.0216(7) Uani 1 1 d . . .
C2 C 0.1514(4) 0.3935(3) 0.1007(2) 0.0226(7) Uani 1 1 d . . .
C3 C 0.2389(5) 0.4245(4) 0.0385(2) 0.0267(8) Uani 1 1 d . . .
H3 H 0.2230 0.4906 0.0088 0.032 Uiso 1 1 calc R . .
C4 C 0.3476(5) 0.3609(4) 0.0198(2) 0.0283(8) Uani 1 1 d . . .
H4 H 0.4027 0.3811 -0.0236 0.034 Uiso 1 1 calc R . .
C5 C 0.3755(5) 0.2674(4) 0.0646(2) 0.0273(8) Uani 1 1 d . . .
H5 H 0.4511 0.2242 0.0523 0.033 Uiso 1 1 calc R . .
C6 C 0.2939(4) 0.2364(3) 0.1276(2) 0.0226(7) Uani 1 1 d . . .
H6 H 0.3150 0.1729 0.1585 0.027 Uiso 1 1 calc R . .
C7 C 0.0452(5) 0.4749(3) 0.1198(2) 0.0255(8) Uani 1 1 d . . .
C8 C -0.1902(6) 0.5085(4) 0.1653(3) 0.0377(10) Uani 1 1 d . . .
H8A H -0.2969 0.4619 0.1724 0.057 Uiso 1 1 calc R . .
H8B H -0.1995 0.5715 0.1289 0.057 Uiso 1 1 calc R . .
H8C H -0.1319 0.5475 0.2160 0.057 Uiso 1 1 calc R . .
C11 C 0.3627(5) 0.1294(4) 0.5202(2) 0.0317(9) Uani 1 1 d . . .
H11 H 0.4520 0.1044 0.5453 0.038 Uiso 1 1 calc R . .
C12 C 0.2385(6) 0.1476(4) 0.5561(2) 0.0339(9) Uani 1 1 d . . .
H12 H 0.2247 0.1372 0.6092 0.041 Uiso 1 1 calc R . .
C13 C 0.1369(5) 0.1843(3) 0.4984(2) 0.0244(7) Uani 1 1 d . . .
C14 C -0.0175(5) 0.2185(4) 0.5060(2) 0.0266(8) Uani 1 1 d . . .
H14 H -0.0869 0.1989 0.4540 0.032 Uiso 1 1 calc R . .
C15 C -0.1051(6) 0.1444(4) 0.5659(3) 0.0393(10) Uani 1 1 d . . .
H15A H -0.2046 0.1684 0.5698 0.059 Uiso 1 1 calc R . .
H15B H -0.0377 0.1601 0.6171 0.059 Uiso 1 1 calc R . .
H15C H -0.1293 0.0569 0.5492 0.059 Uiso 1 1 calc R . .
C16 C 0.0098(6) 0.3545(4) 0.5282(3) 0.0418(11) Uani 1 1 d . . .
H16A H -0.0925 0.3735 0.5327 0.063 Uiso 1 1 calc R . .
H16B H 0.0595 0.4014 0.4876 0.063 Uiso 1 1 calc R . .
H16C H 0.0801 0.3762 0.5785 0.063 Uiso 1 1 calc R . .
C21 C 0.6372(5) 0.3466(4) 0.3598(2) 0.0276(8) Uani 1 1 d . . .
H21 H 0.7355 0.3290 0.3795 0.033 Uiso 1 1 calc R . .
C22 C 0.6180(5) 0.4570(4) 0.3355(2) 0.0308(8) Uani 1 1 d . . .
H22 H 0.6997 0.5293 0.3341 0.037 Uiso 1 1 calc R . .
C23 C 0.4550(5) 0.4420(3) 0.3135(2) 0.0248(8) Uani 1 1 d . . .
C24 C 0.3706(5) 0.5367(3) 0.2857(2) 0.0268(8) Uani 1 1 d . . .
H24 H 0.2612 0.4937 0.2594 0.032 Uiso 1 1 calc R . .
C25 C 0.4583(5) 0.6120(4) 0.2260(3) 0.0369(10) Uani 1 1 d . . .
H25A H 0.4017 0.6734 0.2085 0.055 Uiso 1 1 calc R . .
H25B H 0.4625 0.5576 0.1808 0.055 Uiso 1 1 calc R . .
H25C H 0.5670 0.6530 0.2503 0.055 Uiso 1 1 calc R . .
C26 C 0.3546(6) 0.6198(4) 0.3551(3) 0.0433(11) Uani 1 1 d . . .
H26A H 0.2992 0.6811 0.3359 0.065 Uiso 1 1 calc R . .
H26B H 0.4609 0.6611 0.3825 0.065 Uiso 1 1 calc R . .
H26C H 0.2936 0.5704 0.3913 0.065 Uiso 1 1 calc R . .
C31 C 0.3676(5) -0.0553(4) 0.2847(2) 0.0267(8) Uani 1 1 d . . .
H31 H 0.4574 -0.0875 0.2992 0.032 Uiso 1 1 calc R . .
C32 C 0.2397(5) -0.1076(4) 0.2294(2) 0.0278(8) Uani 1 1 d . . .
H32 H 0.2236 -0.1820 0.1979 0.033 Uiso 1 1 calc R . .
C33 C 0.1374(5) -0.0294(3) 0.2285(2) 0.0227(7) Uani 1 1 d . . .
C34 C -0.0227(5) -0.0457(3) 0.1796(2) 0.0248(8) Uani 1 1 d . . .
H34 H -0.0485 0.0359 0.1778 0.030 Uiso 1 1 calc R . .
C35 C -0.1510(5) -0.1320(4) 0.2166(2) 0.0359(9) Uani 1 1 d . . .
H35A H -0.2549 -0.1416 0.1843 0.054 Uiso 1 1 calc R . .
H35B H -0.1542 -0.0978 0.2693 0.054 Uiso 1 1 calc R . .
H35C H -0.1262 -0.2120 0.2199 0.054 Uiso 1 1 calc R . .
C36 C -0.0188(6) -0.0931(4) 0.0963(2) 0.0352(9) Uani 1 1 d . . .
H36A H -0.1238 -0.1031 0.0650 0.053 Uiso 1 1 calc R . .
H36B H 0.0089 -0.1723 0.0970 0.053 Uiso 1 1 calc R . .
H36C H 0.0611 -0.0346 0.0730 0.053 Uiso 1 1 calc R . .
C41 C -0.1852(4) 0.2995(4) 0.1162(2) 0.0249(8) Uani 1 1 d . . .
C42 C -0.2618(5) 0.2356(4) 0.1733(2) 0.0272(8) Uani 1 1 d . . .
H42 H -0.2573 0.2754 0.2235 0.033 Uiso 1 1 calc R . .
C43 C -0.3433(5) 0.1158(4) 0.1572(3) 0.0358(9) Uani 1 1 d . . .
H43 H -0.3938 0.0725 0.1967 0.043 Uiso 1 1 calc R . .
C44 C -0.3532(5) 0.0568(4) 0.0842(3) 0.0356(9) Uani 1 1 d . . .
H44 H -0.4100 -0.0265 0.0733 0.043 Uiso 1 1 calc R . .
C45 C -0.2785(5) 0.1218(4) 0.0270(3) 0.0349(9) Uani 1 1 d . . .
H45 H -0.2850 0.0823 -0.0234 0.042 Uiso 1 1 calc R . .
C46 C -0.1951(5) 0.2426(4) 0.0425(2) 0.0293(8) Uani 1 1 d . . .
H46 H -0.1450 0.2862 0.0031 0.035 Uiso 1 1 calc R . .
N1 N -0.1037(4) 0.4252(3) 0.13338(18) 0.0275(7) Uani 1 1 d . . .
N11 N 0.1988(4) 0.1865(3) 0.43063(16) 0.0211(6) Uani 1 1 d . . .
N12 N 0.3397(4) 0.1520(3) 0.44529(17) 0.0220(6) Uani 1 1 d . . .
N21 N 0.3791(4) 0.3255(3) 0.32329(17) 0.0218(6) Uani 1 1 d . . .
N22 N 0.4944(4) 0.2684(3) 0.35119(17) 0.0230(6) Uani 1 1 d . . .
N31 N 0.2032(4) 0.0670(3) 0.28105(16) 0.0206(6) Uani 1 1 d . . .
N32 N 0.3448(4) 0.0500(3) 0.31536(17) 0.0237(6) Uani 1 1 d . . .
O1 O 0.0998(3) 0.2682(2) 0.20658(13) 0.0222(5) Uani 1 1 d . . .
O2 O -0.0700(3) 0.1361(2) 0.31560(14) 0.0239(5) Uani 1 1 d . . .
O3 O 0.0831(3) 0.3690(2) 0.35436(15) 0.0264(6) Uani 1 1 d . . .
O4 O 0.0997(4) 0.5868(3) 0.12495(17) 0.0341(6) Uani 1 1 d . . .
B1 B 0.4452(5) 0.1413(4) 0.3811(2) 0.0227(8) Uani 1 1 d . . .
H1 H 0.5413 0.1136 0.4032 0.027 Uiso 1 1 calc R . .
Mo1 Mo 0.10923(3) 0.23659(2) 0.314326(14) 0.01883(11) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 '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 C1 C6 120.7(3) . . ?
O1 C1 C2 119.0(3) . . ?
C6 C1 C2 120.3(3) . . ?
C1 C2 C3 118.1(3) . . ?
C1 C2 C7 124.6(3) . . ?
C3 C2 C7 116.9(3) . . ?
C4 C3 C2 121.4(3) . . ?
C3 C4 C5 119.5(3) . . ?
C4 C5 C6 120.5(4) . . ?
C5 C6 C1 120.1(3) . . ?
O4 C7 N1 121.3(4) . . ?
O4 C7 C2 118.6(4) . . ?
N1 C7 C2 120.0(3) . . ?
N12 C11 C12 109.8(4) . . ?
C11 C12 C13 105.6(3) . . ?
N11 C13 C12 108.7(3) . . ?
N11 C13 C14 123.1(3) . . ?
C12 C13 C14 128.1(3) . . ?
C13 C14 C16 111.5(3) . . ?
C13 C14 C15 111.2(3) . . ?
C16 C14 C15 109.9(3) . . ?
N22 C21 C22 108.2(4) . . ?
C21 C22 C23 106.3(4) . . ?
N21 C23 C22 108.8(3) . . ?
N21 C23 C24 123.6(3) . . ?
C22 C23 C24 127.6(3) . . ?
C23 C24 C25 110.6(3) . . ?
C23 C24 C26 110.5(3) . . ?
C25 C24 C26 110.8(3) . . ?
N32 C31 C32 108.4(3) . . ?
C31 C32 C33 105.9(3) . . ?
N31 C33 C32 109.2(3) . . ?
N31 C33 C34 123.0(3) . . ?
C32 C33 C34 127.8(3) . . ?
C33 C34 C36 110.4(3) . . ?
C33 C34 C35 110.3(3) . . ?
C36 C34 C35 111.0(3) . . ?
C46 C41 C42 120.0(4) . . ?
C46 C41 N1 120.6(3) . . ?
C42 C41 N1 119.3(3) . . ?
C43 C42 C41 120.0(4) . . ?
C42 C43 C44 120.9(4) . . ?
C43 C44 C45 118.8(4) . . ?
C46 C45 C44 121.0(4) . . ?
C45 C46 C41 119.2(4) . . ?
C7 N1 C41 124.8(3) . . ?
C7 N1 C8 117.0(3) . . ?
C41 N1 C8 118.1(3) . . ?
C13 N11 N12 107.4(3) . . ?
C13 N11 Mo1 130.3(3) . . ?
N12 N11 Mo1 122.3(2) . . ?
C11 N12 N11 108.4(3) . . ?
C11 N12 B1 128.8(3) . . ?
N11 N12 B1 122.8(3) . . ?
C23 N21 N22 106.6(3) . . ?
C23 N21 Mo1 129.6(3) . . ?
N22 N21 Mo1 123.3(2) . . ?
C21 N22 N21 110.2(3) . . ?
C21 N22 B1 129.4(3) . . ?
N21 N22 B1 119.3(3) . . ?
C33 N31 N32 106.9(3) . . ?
C33 N31 Mo1 130.3(2) . . ?
N32 N31 Mo1 122.8(2) . . ?
C31 N32 N31 109.7(3) . . ?
C31 N32 B1 130.6(3) . . ?
N31 N32 B1 119.6(3) . . ?
C1 O1 Mo1 147.3(2) . . ?
N32 B1 N22 110.4(3) . . ?
N32 B1 N12 108.0(3) . . ?
N22 B1 N12 106.8(3) . . ?
O3 Mo1 O2 102.97(13) . . ?
O3 Mo1 O1 101.15(12) . . ?
O2 Mo1 O1 102.11(11) . . ?
O3 Mo1 N11 91.04(12) . . ?
O2 Mo1 N11 90.45(12) . . ?
O1 Mo1 N11 159.92(11) . . ?
O3 Mo1 N21 89.56(12) . . ?
O2 Mo1 N21 163.66(11) . . ?
O1 Mo1 N21 85.41(11) . . ?
N11 Mo1 N21 78.72(11) . . ?
O3 Mo1 N31 165.87(12) . . ?
O2 Mo1 N31 86.68(12) . . ?
O1 Mo1 N31 86.64(10) . . ?
N11 Mo1 N31 78.43(10) . . ?
N21 Mo1 N31 79.24(11) . . ?
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
C1 O1 1.361(4) . ?
C1 C6 1.392(5) . ?
C1 C2 1.404(5) . ?
C2 C3 1.407(5) . ?
C2 C7 1.509(5) . ?
C3 C4 1.381(6) . ?
C4 C5 1.384(5) . ?
C5 C6 1.388(5) . ?
C7 O4 1.232(5) . ?
C7 N1 1.343(5) . ?
C8 N1 1.470(5) . ?
C11 N12 1.328(5) . ?
C11 C12 1.369(6) . ?
C12 C13 1.389(5) . ?
C13 N11 1.351(4) . ?
C13 C14 1.508(6) . ?
C14 C16 1.519(6) . ?
C14 C15 1.526(5) . ?
C21 N22 1.330(5) . ?
C21 C22 1.373(6) . ?
C22 C23 1.392(6) . ?
C23 N21 1.352(5) . ?
C23 C24 1.497(5) . ?
C24 C25 1.531(5) . ?
C24 C26 1.531(5) . ?
C31 N32 1.347(5) . ?
C31 C32 1.366(6) . ?
C32 C33 1.397(5) . ?
C33 N31 1.347(5) . ?
C33 C34 1.502(5) . ?
C34 C36 1.521(5) . ?
C34 C35 1.527(5) . ?
C41 C46 1.383(5) . ?
C41 C42 1.395(5) . ?
C41 N1 1.425(5) . ?
C42 C43 1.365(6) . ?
C43 C44 1.382(6) . ?
C44 C45 1.394(6) . ?
C45 C46 1.378(6) . ?
N11 N12 1.374(4) . ?
N11 Mo1 2.204(3) . ?
N12 B1 1.550(5) . ?
N21 N22 1.368(4) . ?
N21 Mo1 2.312(3) . ?
N22 B1 1.528(5) . ?
N31 N32 1.360(4) . ?
N31 Mo1 2.334(3) . ?
N32 B1 1.524(5) . ?
O1 Mo1 1.904(2) . ?
O2 Mo1 1.703(3) . ?
O3 Mo1 1.696(3) . ?
