#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179247 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/67/4316792.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_4316792
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            'C31 H40 B Mo N7 O5'
_chemical_formula_weight         697.45
_chemical_name_common            Tp(iPr)MoO2(OC6H4CONHPh-2)
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.2490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.96030(10)
_cell_length_b                   10.55090(10)
_cell_length_c                   18.2873(2)
_cell_measurement_reflns_used    7936
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      72.9707
_cell_measurement_theta_min      3.5483
_cell_volume                     3272.42(5)
_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)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13544
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         4.84
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.7092
_exptl_absorpt_correction_T_min  0.2599
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+29.0697P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                4824
_reflns_number_total             5813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011428_si_002_1.cif
_cod_data_source_block           jmwng7a
_cod_database_code               4316792
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C31 C 0.8685(4) 0.2574(7) 0.2926(3) 0.0340(16) Uani 1 1 d . . .
H31 H 0.8971 0.3179 0.3206 0.041 Uiso 1 1 calc R . .
C32 C 0.8913(4) 0.1348(7) 0.2786(4) 0.0349(16) Uani 1 1 d . . .
H32 H 0.9383 0.0944 0.2950 0.042 Uiso 1 1 calc R . .
C33 C 0.8328(4) 0.0823(7) 0.2363(3) 0.0300(15) Uani 1 1 d . . .
C34 C 0.8255(4) -0.0536(7) 0.2112(4) 0.0314(15) Uani 1 1 d . . .
H34 H 0.7875 -0.0565 0.1693 0.038 Uiso 1 1 calc R . .
C35 C 0.7921(4) -0.1340(7) 0.2738(4) 0.0380(17) Uani 1 1 d . . .
H35A H 0.7870 -0.2222 0.2577 0.057 Uiso 1 1 calc R . .
H35B H 0.7402 -0.1013 0.2877 0.057 Uiso 1 1 calc R . .
H35C H 0.8278 -0.1298 0.3160 0.057 Uiso 1 1 calc R . .
C36 C 0.9050(5) -0.1057(8) 0.1850(4) 0.046(2) Uani 1 1 d . . .
H36A H 0.8983 -0.1937 0.1689 0.069 Uiso 1 1 calc R . .
H36B H 0.9432 -0.1026 0.2252 0.069 Uiso 1 1 calc R . .
H36C H 0.9241 -0.0543 0.1441 0.069 Uiso 1 1 calc R . .
C21 C 0.7658(4) 0.5408(6) 0.1430(4) 0.0326(15) Uani 1 1 d . . .
H21 H 0.7915 0.6098 0.1665 0.039 Uiso 1 1 calc R . .
C22 C 0.7484(4) 0.5354(6) 0.0705(4) 0.0317(15) Uani 1 1 d . . .
H22 H 0.7584 0.5981 0.0344 0.038 Uiso 1 1 calc R . .
C23 C 0.7126(4) 0.4184(7) 0.0606(3) 0.0292(15) Uani 1 1 d . . .
C24 C 0.6786(4) 0.3623(7) -0.0079(3) 0.0334(16) Uani 1 1 d . . .
H24 H 0.6689 0.2700 0.0006 0.040 Uiso 1 1 calc R . .
C25 C 0.6007(5) 0.4260(10) -0.0240(5) 0.069(3) Uani 1 1 d . . .
H25A H 0.5777 0.3896 -0.0686 0.103 Uiso 1 1 calc R . .
H25B H 0.6092 0.5170 -0.0311 0.103 Uiso 1 1 calc R . .
H25C H 0.5647 0.4126 0.0170 0.103 Uiso 1 1 calc R . .
C26 C 0.7372(5) 0.3764(9) -0.0714(4) 0.056(2) Uani 1 1 d . . .
H26A H 0.7144 0.3389 -0.1158 0.083 Uiso 1 1 calc R . .
H26B H 0.7865 0.3327 -0.0591 0.083 Uiso 1 1 calc R . .
H26C H 0.7479 0.4664 -0.0799 0.083 Uiso 1 1 calc R . .
C11 C 0.6238(4) 0.4092(7) 0.3412(3) 0.0311(15) Uani 1 1 d . . .
H11 H 0.6419 0.4735 0.3735 0.037 Uiso 1 1 calc R . .
C12 C 0.5516(4) 0.3498(8) 0.3447(4) 0.0377(17) Uani 1 1 d . . .
H12 H 0.5114 0.3646 0.3796 0.045 Uiso 1 1 calc R . .
C13 C 0.5493(4) 0.2646(7) 0.2877(3) 0.0328(16) Uani 1 1 d . B .
C14 C 0.4841(4) 0.1780(8) 0.2646(4) 0.0358(17) Uani 1 1 d . . .
H14 H 0.5040 0.0998 0.2399 0.043 Uiso 1 1 calc R A 1
C15 C 0.4350(14) 0.149(4) 0.3292(13) 0.052(8) Uani 0.47(5) 1 d P B 1
H15A H 0.3923 0.0914 0.3149 0.078 Uiso 0.47(5) 1 calc PR B 1
H15B H 0.4125 0.2278 0.3484 0.078 Uiso 0.47(5) 1 calc PR B 1
H15C H 0.4676 0.1088 0.3669 0.078 Uiso 0.47(5) 1 calc PR B 1
C16 C 0.4332(17) 0.266(4) 0.2110(17) 0.048(8) Uani 0.47(5) 1 d P B 1
H16A H 0.4644 0.2863 0.1676 0.072 Uiso 0.47(5) 1 calc PR B 1
H16B H 0.4186 0.3438 0.2364 0.072 Uiso 0.47(5) 1 calc PR B 1
H16C H 0.3853 0.2201 0.1961 0.072 Uiso 0.47(5) 1 calc PR B 1
C15' C 0.460(2) 0.077(4) 0.3266(12) 0.060(10) Uani 0.53(5) 1 d P B 2
H15D H 0.4180 0.0223 0.3083 0.090 Uiso 0.53(5) 1 calc PR B 2
H15E H 0.4425 0.1219 0.3704 0.090 Uiso 0.53(5) 1 calc PR B 2
H15F H 0.5065 0.0248 0.3390 0.090 Uiso 0.53(5) 1 calc PR B 2
C16' C 0.412(2) 0.232(3) 0.236(3) 0.085(13) Uani 0.53(5) 1 d P B 2
H16D H 0.3749 0.1641 0.2237 0.128 Uiso 0.53(5) 1 calc PR B 2
H16E H 0.4232 0.2828 0.1928 0.128 Uiso 0.53(5) 1 calc PR B 2
H16F H 0.3880 0.2866 0.2738 0.128 Uiso 0.53(5) 1 calc PR B 2
C6 C 0.7842(4) -0.0251(6) -0.0176(3) 0.0256(13) Uani 1 1 d . . .
C1 C 0.7216(4) 0.0015(6) 0.0306(3) 0.0240(13) Uani 1 1 d . B .
C2 C 0.6530(4) -0.0701(6) 0.0282(3) 0.0298(15) Uani 1 1 d . . .
H2 H 0.6105 -0.0496 0.0597 0.036 Uiso 1 1 calc R . .
C3 C 0.6462(4) -0.1708(7) -0.0196(3) 0.0352(16) Uani 1 1 d . . .
H3 H 0.5993 -0.2199 -0.0207 0.042 Uiso 1 1 calc R . .
C4 C 0.7086(4) -0.2003(7) -0.0663(4) 0.0358(16) Uani 1 1 d . . .
H4 H 0.7043 -0.2700 -0.0990 0.043 Uiso 1 1 calc R . .
C5 C 0.7758(4) -0.1287(7) -0.0648(3) 0.0344(16) Uani 1 1 d . . .
H5 H 0.8179 -0.1498 -0.0967 0.041 Uiso 1 1 calc R . .
C7 C 0.8602(4) 0.0490(7) -0.0241(3) 0.0283(14) Uani 1 1 d . . .
C41 C 0.9362(4) 0.2224(7) 0.0374(4) 0.0311(15) Uani 1 1 d . . .
C42 C 1.0019(4) 0.2231(8) -0.0070(4) 0.0418(18) Uani 1 1 d . . .
H42 H 1.0077 0.1619 -0.0448 0.050 Uiso 1 1 calc R . .
C43 C 1.0595(4) 0.3151(9) 0.0045(5) 0.051(2) Uani 1 1 d . . .
H43 H 1.1048 0.3170 -0.0259 0.061 Uiso 1 1 calc R . .
C44 C 1.0514(5) 0.4041(8) 0.0599(5) 0.049(2) Uani 1 1 d . . .
H44 H 1.0908 0.4669 0.0672 0.059 Uiso 1 1 calc R . .
C45 C 0.9855(5) 0.4008(9) 0.1044(5) 0.050(2) Uani 1 1 d . . .
H45 H 0.9797 0.4611 0.1426 0.060 Uiso 1 1 calc R . .
C46 C 0.9282(4) 0.3099(7) 0.0933(4) 0.0371(17) Uani 1 1 d . . .
H46 H 0.8832 0.3073 0.1240 0.045 Uiso 1 1 calc R . .
B1 B 0.7476(4) 0.3958(8) 0.2568(4) 0.0305(17) Uani 1 1 d . . .
H1 H 0.7712 0.4650 0.2872 0.037 Uiso 1 1 calc R . .
N1 N 0.8741(3) 0.1337(5) 0.0302(3) 0.0313(13) Uani 1 1 d . . .
H H 0.8396 0.1335 0.0660 0.038 Uiso 1 1 calc R . .
N31 N 0.7760(3) 0.1681(5) 0.2241(3) 0.0262(11) Uani 1 1 d . . .
N32 N 0.7990(3) 0.2764(5) 0.2597(3) 0.0272(12) Uani 1 1 d . . .
N21 N 0.7091(3) 0.3561(5) 0.1258(3) 0.0240(11) Uani 1 1 d . . .
N22 N 0.7419(3) 0.4360(5) 0.1763(3) 0.0278(12) Uani 1 1 d . . .
N11 N 0.6193(3) 0.2696(5) 0.2505(3) 0.0255(11) Uani 1 1 d . . .
N12 N 0.6644(3) 0.3610(6) 0.2843(3) 0.0292(13) Uani 1 1 d . B .
O3 O 0.5774(3) 0.1911(5) 0.1082(2) 0.0327(11) Uani 1 1 d . . .
O2 O 0.6380(3) 0.0219(5) 0.1991(2) 0.0370(12) Uani 1 1 d . . .
O1 O 0.7284(3) 0.0978(4) 0.0791(2) 0.0284(10) Uani 1 1 d . . .
O4 O 0.9052(3) 0.0314(5) -0.0760(2) 0.0371(12) Uani 1 1 d . . .
O5 O 0.9271(7) -0.1085(13) -0.2083(7) 0.173(5) Uani 1 1 d . . .
Mo1 Mo 0.65953(3) 0.16050(5) 0.15727(3) 0.02406(16) Uani 1 1 d . B .
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'
B B 0.0090 0.0039 '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'
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
N32 C31 C32 107.8(6) . . ?
C33 C32 C31 106.3(6) . . ?
N31 C33 C32 109.8(6) . . ?
N31 C33 C34 122.2(6) . . ?
C32 C33 C34 127.8(6) . . ?
C33 C34 C36 111.4(6) . . ?
C33 C34 C35 109.1(5) . . ?
C36 C34 C35 111.2(6) . . ?
N22 C21 C22 110.3(6) . . ?
C21 C22 C23 105.0(6) . . ?
N21 C23 C22 109.6(6) . . ?
N21 C23 C24 121.5(6) . . ?
C22 C23 C24 128.9(6) . . ?
C23 C24 C25 108.7(6) . . ?
C23 C24 C26 110.2(6) . . ?
C25 C24 C26 112.1(7) . . ?
N12 C11 C12 108.7(6) . . ?
C11 C12 C13 106.6(6) . . ?
N11 C13 C12 109.1(6) . . ?
N11 C13 C14 121.6(6) . . ?
C12 C13 C14 129.2(6) . . ?
C16' C14 C15 83.4(17) . . ?
C16' C14 C13 119.0(12) . . ?
C15 C14 C13 108.6(11) . . ?
C16' C14 C16 25.5(16) . . ?
C15 C14 C16 107.7(15) . . ?
C13 C14 C16 102.6(14) . . ?
C16' C14 C15' 107.4(14) . . ?
C15 C14 C15' 32.6(10) . . ?
C13 C14 C15' 113.1(8) . . ?
C16 C14 C15' 132.8(13) . . ?
C5 C6 C1 117.8(6) . . ?
C5 C6 C7 116.1(6) . . ?
C1 C6 C7 126.1(6) . . ?
O1 C1 C2 119.9(6) . . ?
O1 C1 C6 119.8(6) . . ?
C2 C1 C6 120.3(6) . . ?
C3 C2 C1 120.5(6) . . ?
C2 C3 C4 119.8(7) . . ?
C5 C4 C3 119.9(7) . . ?
C4 C5 C6 121.7(6) . . ?
O4 C7 N1 123.8(6) . . ?
O4 C7 C6 120.8(6) . . ?
N1 C7 C6 115.4(5) . . ?
C42 C41 C46 120.8(7) . . ?
C42 C41 N1 123.5(7) . . ?
C46 C41 N1 115.7(6) . . ?
C41 C42 C43 118.8(8) . . ?
C44 C43 C42 120.7(7) . . ?
C45 C44 C43 119.6(8) . . ?
C46 C45 C44 120.0(8) . . ?
C45 C46 C41 120.1(7) . . ?
N32 B1 N22 107.1(5) . . ?
N32 B1 N12 108.3(6) . . ?
N22 B1 N12 108.9(5) . . ?
C7 N1 C41 129.1(6) . . ?
C33 N31 N32 106.3(5) . . ?
C33 N31 Mo1 132.4(5) . . ?
N32 N31 Mo1 121.3(4) . . ?
C31 N32 N31 109.7(6) . . ?
C31 N32 B1 129.7(6) . . ?
N31 N32 B1 120.5(5) . . ?
C23 N21 N22 105.9(5) . . ?
C23 N21 Mo1 131.9(4) . . ?
N22 N21 Mo1 122.2(4) . . ?
C21 N22 N21 109.2(5) . . ?
C21 N22 B1 130.7(6) . . ?
N21 N22 B1 120.1(5) . . ?
C13 N11 N12 106.6(5) . . ?
C13 N11 Mo1 130.2(5) . . ?
N12 N11 Mo1 123.2(4) . . ?
C11 N12 N11 109.0(5) . . ?
C11 N12 B1 129.2(6) . . ?
N11 N12 B1 121.8(5) . . ?
C1 O1 Mo1 132.9(4) . . ?
O3 Mo1 O2 103.1(2) . . ?
O3 Mo1 O1 99.8(2) . . ?
O2 Mo1 O1 99.7(2) . . ?
O3 Mo1 N11 93.1(2) . . ?
O2 Mo1 N11 92.0(2) . . ?
O1 Mo1 N11 160.10(19) . . ?
O3 Mo1 N21 89.8(2) . . ?
O2 Mo1 N21 165.5(2) . . ?
O1 Mo1 N21 84.34(18) . . ?
N11 Mo1 N21 80.62(19) . . ?
O3 Mo1 N31 166.9(2) . . ?
O2 Mo1 N31 88.7(2) . . ?
O1 Mo1 N31 83.54(18) . . ?
N11 Mo1 N31 80.64(18) . . ?
N21 Mo1 N31 77.86(19) . . ?
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
C31 N32 1.337(8) . ?
C31 C32 1.374(10) . ?
C32 C33 1.372(10) . ?
C33 N31 1.341(8) . ?
C33 C34 1.511(10) . ?
C34 C36 1.533(9) . ?
C34 C35 1.536(9) . ?
C21 N22 1.327(8) . ?
C21 C22 1.359(10) . ?
C22 C23 1.387(9) . ?
C23 N21 1.364(8) . ?
C23 C24 1.498(9) . ?
C24 C25 1.510(10) . ?
C24 C26 1.539(10) . ?
C11 N12 1.351(8) . ?
C11 C12 1.376(10) . ?
C12 C13 1.377(10) . ?
C13 N11 1.371(8) . ?
C13 C14 1.493(10) . ?
C14 C16' 1.45(3) . ?
C14 C15 1.48(2) . ?
C14 C16 1.60(4) . ?
C14 C15' 1.610(19) . ?
C6 C5 1.400(9) . ?
C6 C1 1.411(8) . ?
C6 C7 1.513(9) . ?
C1 O1 1.354(7) . ?
C1 C2 1.387(9) . ?
C2 C3 1.380(9) . ?
C3 C4 1.398(10) . ?
C4 C5 1.368(10) . ?
C7 O4 1.234(8) . ?
C7 N1 1.356(8) . ?
C41 C42 1.382(10) . ?
C41 C46 1.385(10) . ?
C41 N1 1.414(8) . ?
C42 C43 1.393(11) . ?
C43 C44 1.388(12) . ?
C44 C45 1.387(12) . ?
C45 C46 1.380(10) . ?
B1 N32 1.532(10) . ?
B1 N22 1.534(9) . ?
B1 N12 1.545(9) . ?
N31 N32 1.370(7) . ?
N31 Mo1 2.319(5) . ?
N21 N22 1.367(7) . ?
N21 Mo1 2.302(5) . ?
N11 N12 1.376(7) . ?
N11 Mo1 2.170(5) . ?
O3 Mo1 1.684(4) . ?
O2 Mo1 1.691(5) . ?
O1 Mo1 1.965(4) . ?
