#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:17:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179406 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/03/4330398.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_4330398
loop_
_publ_author_name
'Martina E. Judmaier'
'Christof Holzer'
'Manuel Volpe'
'Nadia C. Mösch-Zanetti'
_publ_section_title
;
 Molybdenum(VI) Dioxo Complexes Employing Schiff Base Ligands with an
 Intramolecular Donor for Highly Selective Olefin Epoxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9956
_journal_page_last               9966
_journal_paper_doi               10.1021/ic301464w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C38 H62 Mo N4 O4'
_chemical_formula_weight         734.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 98.025(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.606(2)
_cell_length_b                   6.8112(7)
_cell_length_c                   15.1333(16)
_cell_measurement_reflns_used    4245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.65
_cell_volume                     2001.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58693
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         2.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       tablet
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.254
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0478
_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)+(0.0787P)²+10.4329P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                2076
_reflns_number_total             2133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301464w_si_002.cif
_cod_data_source_block           mobuim
_cod_database_code               4330398
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Mo1 Mo 0.5000 0.8056 1.0000 0.0111(2) Uani 1 2 d S
N1 N 0.4297(3) 1.0810(8) 1.0046(3) 0.0117(10) Uiso 1 1 d .
N2 N 0.2831(4) 1.2037(13) 0.9176(5) 0.0233(17) Uani 1 1 d .
O1 O 0.5705(2) 0.6559(7) 1.0027(3) 0.0198(10) Uani 1 1 d .
O2 O 0.5122(2) 0.8521(5) 1.1279(3) 0.0127(9) Uiso 1 1 d .
C1 C 0.4075(3) 1.1416(9) 1.0758(4) 0.0159(12) Uani 1 1 d .
H1 H 0.3805 1.2580 1.0703 0.019 Uiso 1 1 calc R
C2 C 0.4193(3) 1.0513(10) 1.1639(4) 0.0167(13) Uani 1 1 d .
C3 C 0.3787(3) 1.1169(10) 1.2277(4) 0.0183(13) Uani 1 1 d .
H3 H 0.3451 1.2160 1.2118 0.022 Uiso 1 1 calc R
C4 C 0.3868(3) 1.0402(11) 1.3128(4) 0.0218(14) Uani 1 1 d .
C5 C 0.4365(3) 0.8952(11) 1.3329(4) 0.0222(14) Uani 1 1 d .
H5 H 0.4416 0.8397 1.3910 0.027 Uiso 1 1 calc R
C6 C 0.4798(3) 0.8252(17) 1.2734(4) 0.0190(16) Uani 1 1 d .
C7 C 0.4699(3) 0.9058(9) 1.1869(4) 0.0140(12) Uani 1 1 d .
C8 C 0.3426(4) 1.1042(13) 1.3833(5) 0.0275(16) Uani 1 1 d .
C9 C 0.2985(4) 1.283(2) 1.3531(5) 0.040(2) Uani 1 1 d .
H9A H 0.3285 1.3945 1.3444 0.059 Uiso 1 1 calc R
H9B H 0.2695 1.3163 1.3986 0.059 Uiso 1 1 calc R
H9C H 0.2693 1.2532 1.2967 0.059 Uiso 1 1 calc R
C10 C 0.2947(4) 0.9341(16) 1.4015(5) 0.042(2) Uani 1 1 d .
H10A H 0.2664 0.9744 1.4468 0.063 Uiso 1 1 calc R
H10B H 0.3225 0.8196 1.4229 0.063 Uiso 1 1 calc R
H10C H 0.2648 0.9002 1.3462 0.063 Uiso 1 1 calc R
C11 C 0.3895(4) 1.1556(15) 1.4710(5) 0.038(2) Uani 1 1 d .
H11A H 0.4201 1.2642 1.4603 0.056 Uiso 1 1 calc R
H11B H 0.4172 1.0406 1.4919 0.056 Uiso 1 1 calc R
H11C H 0.3610 1.1945 1.5163 0.056 Uiso 1 1 calc R
C12 C 0.5336(4) 0.6668(11) 1.2995(4) 0.0241(15) Uani 1 1 d .
C13 C 0.6068(4) 0.7448(14) 1.2900(5) 0.037(2) Uani 1 1 d .
H13A H 0.6153 0.8668 1.3241 0.056 Uiso 1 1 calc R
H13B H 0.6098 0.7703 1.2269 0.056 Uiso 1 1 calc R
H13C H 0.6413 0.6465 1.3129 0.056 Uiso 1 1 calc R
C14 C 0.5177(5) 0.4850(12) 1.2415(5) 0.0367(19) Uani 1 1 d .
H14A H 0.5538 0.3866 1.2571 0.055 Uiso 1 1 calc R
H14B H 0.5158 0.5211 1.1785 0.055 Uiso 1 1 calc R
H14C H 0.4732 0.4306 1.2516 0.055 Uiso 1 1 calc R
C15 C 0.5359(5) 0.6025(14) 1.3969(5) 0.0366(19) Uani 1 1 d .
H15A H 0.5458 0.7163 1.4361 0.055 Uiso 1 1 calc R
H15B H 0.5720 0.5035 1.4113 0.055 Uiso 1 1 calc R
H15C H 0.4912 0.5464 1.4055 0.055 Uiso 1 1 calc R
C16 C 0.4104(3) 1.1981(9) 0.9242(4) 0.0141(12) Uani 1 1 d .
H16A H 0.4461 1.1847 0.8843 0.017 Uiso 1 1 calc R
H16B H 0.4077 1.3383 0.9406 0.017 Uiso 1 1 calc R
C17 C 0.3407(3) 1.1310(10) 0.8749(4) 0.0166(13) Uani 1 1 d .
H17A H 0.3357 1.1788 0.8125 0.020 Uiso 1 1 calc R
H17B H 0.3393 0.9857 0.8733 0.020 Uiso 1 1 calc R
C18 C 0.2205(4) 1.0958(16) 0.8850(6) 0.040(2) Uani 1 1 d .
H18A H 0.2117 1.1040 0.8197 0.060 Uiso 1 1 calc R
H18B H 0.1816 1.1529 0.9102 0.060 Uiso 1 1 calc R
H18C H 0.2260 0.9580 0.9031 0.060 Uiso 1 1 calc R
C19 C 0.2717(6) 1.4119(16) 0.8978(7) 0.030(2) Uani 1 1 d .
H19A H 0.3143 1.4851 0.9166 0.045 Uiso 1 1 calc R
H19B H 0.2351 1.4613 0.9299 0.045 Uiso 1 1 calc R
H19C H 0.2580 1.4292 0.8334 0.045 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
Mo Mo -1.6832 0.6857 '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'
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'
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
O1 Mo1 O1 107.0(3) . 2_657
O1 Mo1 O2 94.96(19) . .
O1 Mo1 O2 96.18(19) 2_657 .
O1 Mo1 O2 96.18(19) . 2_657
O1 Mo1 O2 94.96(19) 2_657 2_657
O2 Mo1 O2 161.2(2) . 2_657
O1 Mo1 N1 90.1(2) . 2_657
O1 Mo1 N1 162.8(2) 2_657 2_657
O2 Mo1 N1 84.70(16) . 2_657
O2 Mo1 N1 80.23(16) 2_657 2_657
O1 Mo1 N1 162.8(2) . .
O1 Mo1 N1 90.1(2) 2_657 .
O2 Mo1 N1 80.23(16) . .
O2 Mo1 N1 84.70(16) 2_657 .
N1 Mo1 N1 73.1(3) 2_657 .
C1 N1 C16 116.4(5) . .
C1 N1 Mo1 123.7(4) . .
C16 N1 Mo1 120.0(4) . .
C18 N2 C19 108.8(8) . .
C18 N2 C17 110.2(7) . .
C19 N2 C17 110.1(9) . .
C7 O2 Mo1 134.5(4) . .
N1 C1 C2 127.1(6) . .
C3 C2 C7 120.0(6) . .
C3 C2 C1 117.5(6) . .
C7 C2 C1 122.5(6) . .
C4 C3 C2 121.2(6) . .
C3 C4 C5 117.3(6) . .
C3 C4 C8 122.8(7) . .
C5 C4 C8 119.8(6) . .
C4 C5 C6 124.6(7) . .
C5 C6 C7 116.5(8) . .
C5 C6 C12 122.2(6) . .
C7 C6 C12 121.2(6) . .
O2 C7 C6 119.4(6) . .
O2 C7 C2 120.2(5) . .
C6 C7 C2 120.2(6) . .
C9 C8 C4 111.7(6) . .
C9 C8 C10 108.6(7) . .
C4 C8 C10 109.2(6) . .
C9 C8 C11 108.7(7) . .
C4 C8 C11 109.7(6) . .
C10 C8 C11 108.8(7) . .
C6 C12 C14 110.3(6) . .
C6 C12 C15 112.2(6) . .
C14 C12 C15 107.3(6) . .
C6 C12 C13 110.4(6) . .
C14 C12 C13 110.0(7) . .
C15 C12 C13 106.5(6) . .
N1 C16 C17 110.6(5) . .
N2 C17 C16 112.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O1 1.714(4) .
Mo1 O1 1.714(4) 2_657
Mo1 O2 1.942(4) .
Mo1 O2 1.942(4) 2_657
Mo1 N1 2.334(5) 2_657
Mo1 N1 2.334(5) .
N1 C1 1.285(8) .
N1 C16 1.461(7) .
N2 C18 1.457(11) .
N2 C19 1.460(10) .
N2 C17 1.464(9) .
O2 C7 1.352(7) .
C1 C2 1.458(9) .
C2 C3 1.405(9) .
C2 C7 1.412(9) .
C3 C4 1.378(10) .
C4 C5 1.391(11) .
C4 C8 1.529(9) .
C5 C6 1.404(9) .
C6 C7 1.408(9) .
C6 C12 1.522(11) .
C8 C9 1.527(15) .
C8 C10 1.540(12) .
C8 C11 1.544(10) .
C12 C14 1.525(11) .
C12 C15 1.532(9) .
C12 C13 1.554(10) .
C16 C17 1.533(8) .
