#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179247 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/67/4316794.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_4316794
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 O5'
_chemical_formula_weight         709.46
_chemical_name_common            Tp(iPr)MoO2(OC6H4CONH(C6H4OMe-4)-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                 94.431(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5817(2)
_cell_length_b                   13.2801(3)
_cell_length_c                   29.2857(5)
_cell_measurement_temperature    130(2)
_cell_volume                     3327.59(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            12857
_diffrn_reflns_theta_full        73.04
_diffrn_reflns_theta_max         73.04
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    3.639
_exptl_absorpt_correction_T_max  0.7847
_exptl_absorpt_correction_T_min  0.4754
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0470
_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)+(0.0147P)²+17.9226P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                5539
_reflns_number_total             6495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1011428_si_002_3.cif
_cod_data_source_block           jmwng19
_cod_database_code               4316794
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
C1 C 0.3083(5) 0.8325(3) 0.15326(15) 0.0176(9) Uani 1 1 d . . .
C2 C 0.2502(5) 0.9312(4) 0.15632(15) 0.0218(10) Uani 1 1 d . . .
C3 C 0.3489(6) 1.0038(4) 0.17788(18) 0.0283(11) Uani 1 1 d . . .
H3 H 0.3117 1.0707 0.1807 0.034 Uiso 1 1 calc R . .
C4 C 0.4983(7) 0.9808(4) 0.19514(19) 0.0351(13) Uani 1 1 d . . .
H4 H 0.5624 1.0311 0.2100 0.042 Uiso 1 1 calc R . .
C5 C 0.5546(6) 0.8840(4) 0.19072(17) 0.0294(11) Uani 1 1 d . . .
H5 H 0.6582 0.8681 0.2022 0.035 Uiso 1 1 calc R . .
C6 C 0.4606(6) 0.8100(4) 0.16966(16) 0.0250(10) Uani 1 1 d . . .
H6 H 0.5004 0.7438 0.1664 0.030 Uiso 1 1 calc R . .
C7 C 0.0926(6) 0.9681(4) 0.13770(16) 0.0225(10) Uani 1 1 d . . .
C8 C -0.7015(6) 1.0357(4) 0.04453(19) 0.0347(13) Uani 1 1 d . . .
H8A H -0.8093 1.0283 0.0313 0.052 Uiso 1 1 calc R . .
H8B H -0.6443 1.0808 0.0253 0.052 Uiso 1 1 calc R . .
H8C H -0.7018 1.0639 0.0754 0.052 Uiso 1 1 calc R . .
C41 C -0.1667(5) 0.9155(3) 0.10201(16) 0.0200(9) Uani 1 1 d . . .
C42 C -0.2525(6) 0.8316(3) 0.08661(16) 0.0224(10) Uani 1 1 d . . .
H42 H -0.2055 0.7668 0.0886 0.027 Uiso 1 1 calc R . .
C43 C -0.4052(6) 0.8413(4) 0.06844(17) 0.0253(10) Uani 1 1 d . . .
H43 H -0.4629 0.7832 0.0586 0.030 Uiso 1 1 calc R . .
C44 C -0.4749(6) 0.9364(4) 0.06456(16) 0.0236(10) Uani 1 1 d . . .
C45 C -0.3889(6) 1.0202(4) 0.07911(17) 0.0268(11) Uani 1 1 d . . .
H45 H -0.4352 1.0851 0.0763 0.032 Uiso 1 1 calc R . .
C46 C -0.2357(6) 1.0104(4) 0.09771(18) 0.0282(11) Uani 1 1 d . . .
H46 H -0.1779 1.0686 0.1075 0.034 Uiso 1 1 calc R . .
N1 N -0.0117(4) 0.8984(3) 0.12082(14) 0.0236(9) Uani 1 1 d . . .
H H 0.0203 0.8354 0.1216 0.028 Uiso 1 1 calc R . .
O1 O 0.2135(4) 0.7591(2) 0.13354(11) 0.0219(7) Uani 1 1 d . . .
O2 O 0.3577(4) 0.5928(2) 0.09422(11) 0.0236(7) Uani 1 1 d . . .
O3 O 0.3259(4) 0.5919(2) 0.18381(11) 0.0223(7) Uani 1 1 d . . .
O4 O 0.0641(4) 1.0592(3) 0.13806(15) 0.0375(9) Uani 1 1 d . . .
O5 O -0.6269(4) 0.9389(3) 0.04681(13) 0.0320(8) Uani 1 1 d . . .
C11 C -0.0148(6) 0.3270(3) 0.12255(15) 0.0204(9) Uani 1 1 d . . .
H11 H -0.1089 0.2892 0.1190 0.024 Uiso 1 1 calc R . .
C12 C 0.1337(6) 0.2861(3) 0.12848(15) 0.0204(9) Uani 1 1 d . . .
H12 H 0.1619 0.2169 0.1300 0.024 Uiso 1 1 calc R . .
C13 C 0.2330(5) 0.3700(3) 0.13172(15) 0.0200(9) Uani 1 1 d . . .
C14 C 0.4088(5) 0.3701(4) 0.13915(17) 0.0241(10) Uani 1 1 d . . .
H14 H 0.4489 0.4365 0.1290 0.029 Uiso 1 1 calc R . .
C15 C 0.4776(7) 0.2880(5) 0.1115(2) 0.0463(16) Uani 1 1 d . . .
H15A H 0.5918 0.2891 0.1168 0.070 Uiso 1 1 calc R . .
H15B H 0.4478 0.2989 0.0789 0.070 Uiso 1 1 calc R . .
H15C H 0.4381 0.2225 0.1209 0.070 Uiso 1 1 calc R . .
C16 C 0.4573(7) 0.3564(5) 0.1904(2) 0.0432(15) Uani 1 1 d . . .
H16A H 0.5716 0.3564 0.1953 0.065 Uiso 1 1 calc R . .
H16B H 0.4163 0.2923 0.2010 0.065 Uiso 1 1 calc R . .
H16C H 0.4149 0.4119 0.2078 0.065 Uiso 1 1 calc R . .
C21 C -0.2501(6) 0.5929(4) 0.18455(18) 0.0280(11) Uani 1 1 d . . .
H21 H -0.3536 0.5670 0.1815 0.034 Uiso 1 1 calc R . .
C22 C -0.1903(6) 0.6563(4) 0.21865(18) 0.0303(11) Uani 1 1 d . . .
H22 H -0.2433 0.6830 0.2433 0.036 Uiso 1 1 calc R . .
C23 C -0.0355(5) 0.6731(4) 0.20945(16) 0.0218(10) Uani 1 1 d . . .
C24 C 0.0857(6) 0.7335(4) 0.23813(16) 0.0247(10) Uani 1 1 d . . .
H24 H 0.1769 0.7451 0.2195 0.030 Uiso 1 1 calc R . .
C25 C 0.1419(7) 0.6719(5) 0.28037(18) 0.0358(13) Uani 1 1 d . . .
H25A H 0.2205 0.7105 0.2991 0.054 Uiso 1 1 calc R . .
H25B H 0.1882 0.6087 0.2707 0.054 Uiso 1 1 calc R . .
H25C H 0.0531 0.6571 0.2984 0.054 Uiso 1 1 calc R . .
C26 C 0.0218(7) 0.8359(4) 0.25148(18) 0.0318(12) Uani 1 1 d . . .
H26A H 0.1030 0.8729 0.2699 0.048 Uiso 1 1 calc R . .
H26B H -0.0690 0.8261 0.2693 0.048 Uiso 1 1 calc R . .
H26C H -0.0095 0.8744 0.2237 0.048 Uiso 1 1 calc R . .
C31 C -0.1839(6) 0.5774(4) 0.03164(17) 0.0294(11) Uani 1 1 d . . .
H31 H -0.2802 0.5450 0.0227 0.035 Uiso 1 1 calc R . .
C32 C -0.1054(6) 0.6399(4) 0.00484(17) 0.0300(12) Uani 1 1 d . . .
H32 H -0.1352 0.6594 -0.0258 0.036 Uiso 1 1 calc R . .
C33 C 0.0284(6) 0.6697(3) 0.03169(16) 0.0218(10) Uani 1 1 d . . .
C34 C 0.1524(6) 0.7424(4) 0.01915(16) 0.0248(10) Uani 1 1 d . . .
H34 H 0.2069 0.7686 0.0482 0.030 Uiso 1 1 calc R . .
C35 C 0.2742(6) 0.6928(4) -0.00864(18) 0.0320(12) Uani 1 1 d . . .
H35A H 0.3527 0.7427 -0.0159 0.048 Uiso 1 1 calc R . .
H35B H 0.2232 0.6657 -0.0371 0.048 Uiso 1 1 calc R . .
H35C H 0.3252 0.6379 0.0092 0.048 Uiso 1 1 calc R . .
C36 C 0.0761(7) 0.8322(4) -0.00721(17) 0.0300(11) Uani 1 1 d . . .
H36A H 0.1573 0.8795 -0.0152 0.045 Uiso 1 1 calc R . .
H36B H 0.0038 0.8662 0.0120 0.045 Uiso 1 1 calc R . .
H36C H 0.0186 0.8079 -0.0353 0.045 Uiso 1 1 calc R . .
N11 N 0.1468(4) 0.4554(3) 0.12796(13) 0.0169(8) Uani 1 1 d . . .
N12 N -0.0067(4) 0.4262(3) 0.12258(13) 0.0199(8) Uani 1 1 d . . .
N21 N -0.0043(4) 0.6240(3) 0.17142(13) 0.0208(8) Uani 1 1 d . . .
N22 N -0.1376(4) 0.5739(3) 0.15630(14) 0.0221(8) Uani 1 1 d . . .
N31 N 0.0290(4) 0.6259(3) 0.07300(13) 0.0201(8) Uani 1 1 d . . .
N32 N -0.1043(4) 0.5687(3) 0.07276(14) 0.0223(8) Uani 1 1 d . . .
Mo1 Mo 0.22342(4) 0.61334(3) 0.132775(12) 0.01621(10) Uani 1 1 d . . .
B1 B -0.1398(6) 0.5044(4) 0.11427(19) 0.0235(11) Uani 1 1 d . . .
H1 H -0.2433 0.4702 0.1089 0.028 Uiso 1 1 calc R . .
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'
Mo Mo -0.0483 2.7339 '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'
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 120.4(4) . . ?
O1 C1 C2 119.2(4) . . ?
C6 C1 C2 120.4(4) . . ?
C3 C2 C1 117.7(4) . . ?
C3 C2 C7 115.9(4) . . ?
C1 C2 C7 126.4(4) . . ?
C4 C3 C2 121.8(5) . . ?
C3 C4 C5 119.6(5) . . ?
C4 C5 C6 120.4(5) . . ?
C5 C6 C1 120.1(5) . . ?
O4 C7 N1 123.1(5) . . ?
O4 C7 C2 119.4(4) . . ?
N1 C7 C2 117.5(4) . . ?
C42 C41 C46 119.0(4) . . ?
C42 C41 N1 117.0(4) . . ?
C46 C41 N1 124.0(4) . . ?
C43 C42 C41 120.8(4) . . ?
C42 C43 C44 120.2(4) . . ?
O5 C44 C45 124.6(4) . . ?
O5 C44 C43 116.2(4) . . ?
C45 C44 C43 119.1(4) . . ?
C44 C45 C46 120.8(5) . . ?
C45 C46 C41 120.1(5) . . ?
C7 N1 C41 127.3(4) . . ?
C1 O1 Mo1 133.7(3) . . ?
C44 O5 C8 116.6(4) . . ?
N12 C11 C12 110.1(4) . . ?
C11 C12 C13 104.2(4) . . ?
N11 C13 C12 109.6(4) . . ?
N11 C13 C14 123.1(4) . . ?
C12 C13 C14 127.3(4) . . ?
C15 C14 C13 110.6(4) . . ?
C15 C14 C16 110.6(5) . . ?
C13 C14 C16 109.4(4) . . ?
N22 C21 C22 108.5(4) . . ?
C21 C22 C23 105.4(4) . . ?
N21 C23 C22 109.8(4) . . ?
N21 C23 C24 123.2(4) . . ?
C22 C23 C24 127.0(4) . . ?
C23 C24 C26 111.6(4) . . ?
C23 C24 C25 109.0(4) . . ?
C26 C24 C25 111.5(4) . . ?
N32 C31 C32 109.3(4) . . ?
C31 C32 C33 105.7(4) . . ?
N31 C33 C32 109.3(4) . . ?
N31 C33 C34 123.0(4) . . ?
C32 C33 C34 127.6(4) . . ?
C33 C34 C35 112.4(4) . . ?
C33 C34 C36 109.8(4) . . ?
C35 C34 C36 110.5(4) . . ?
C13 N11 N12 106.6(3) . . ?
C13 N11 Mo1 129.4(3) . . ?
N12 N11 Mo1 123.9(3) . . ?
C11 N12 N11 109.4(4) . . ?
C11 N12 B1 129.2(4) . . ?
N11 N12 B1 121.2(4) . . ?
C23 N21 N22 106.9(4) . . ?
C23 N21 Mo1 131.5(3) . . ?
N22 N21 Mo1 121.6(3) . . ?
C21 N22 N21 109.4(4) . . ?
C21 N22 B1 129.9(4) . . ?
N21 N22 B1 120.6(4) . . ?
C33 N31 N32 106.8(4) . . ?
C33 N31 Mo1 131.4(3) . . ?
N32 N31 Mo1 120.8(3) . . ?
C31 N32 N31 108.8(4) . . ?
C31 N32 B1 129.8(4) . . ?
N31 N32 B1 121.3(4) . . ?
O2 Mo1 O3 103.09(16) . . ?
O2 Mo1 O1 101.58(15) . . ?
O3 Mo1 O1 100.20(14) . . ?
O2 Mo1 N11 91.09(15) . . ?
O3 Mo1 N11 91.65(15) . . ?
O1 Mo1 N11 160.09(14) . . ?
O2 Mo1 N31 89.71(15) . . ?
O3 Mo1 N31 164.92(14) . . ?
O1 Mo1 N31 84.71(13) . . ?
N11 Mo1 N31 80.03(14) . . ?
O2 Mo1 N21 165.56(14) . . ?
O3 Mo1 N21 88.83(14) . . ?
O1 Mo1 N21 83.97(14) . . ?
N11 Mo1 N21 80.31(14) . . ?
N31 Mo1 N21 77.44(13) . . ?
N32 B1 N22 108.0(4) . . ?
N32 B1 N12 108.0(4) . . ?
N22 B1 N12 108.3(4) . . ?
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 1.368(5) . ?
C1 C6 1.390(6) . ?
C1 C2 1.408(7) . ?
C2 C3 1.400(6) . ?
C2 C7 1.501(7) . ?
C3 C4 1.375(8) . ?
C4 C5 1.383(8) . ?
C5 C6 1.385(7) . ?
C7 O4 1.235(6) . ?
C7 N1 1.354(6) . ?
C8 O5 1.435(6) . ?
C41 C42 1.392(6) . ?
C41 C46 1.394(7) . ?
C41 N1 1.418(6) . ?
C42 C43 1.382(7) . ?
C43 C44 1.399(7) . ?
C44 O5 1.366(6) . ?
C44 C45 1.384(7) . ?
C45 C46 1.390(7) . ?
O1 Mo1 1.938(3) . ?
O2 Mo1 1.696(3) . ?
O3 Mo1 1.699(3) . ?
C11 N12 1.319(6) . ?
C11 C12 1.384(7) . ?
C12 C13 1.403(6) . ?
C13 N11 1.354(6) . ?
C13 C14 1.508(6) . ?
C14 C15 1.506(7) . ?
C14 C16 1.538(7) . ?
C21 N22 1.343(6) . ?
C21 C22 1.375(7) . ?
C22 C23 1.394(7) . ?
C23 N21 1.336(6) . ?
C23 C24 1.515(6) . ?
C24 C26 1.529(7) . ?
C24 C25 1.529(7) . ?
C31 N32 1.343(6) . ?
C31 C32 1.356(7) . ?
C32 C33 1.398(7) . ?
C33 N31 1.342(6) . ?
C33 C34 1.504(7) . ?
C34 C35 1.524(7) . ?
C34 C36 1.539(7) . ?
N11 N12 1.371(5) . ?
N11 Mo1 2.199(3) . ?
N12 B1 1.549(6) . ?
N21 N22 1.368(5) . ?
N21 Mo1 2.337(4) . ?
N22 B1 1.537(7) . ?
N31 N32 1.373(5) . ?
N31 Mo1 2.329(4) . ?
N32 B1 1.535(7) . ?
