#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:52:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179159 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/20/4312045.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_4312045
loop_
_publ_author_name
'Justin T. Hoffman'
'Simon Einwaechter'
'Balwant S. Chohan'
'Partha Basu'
'Carl J. Carrano'
_publ_section_title
;
 Isomerization and Oxygen Atom Transfer Reactivity in Oxo-Mo Complexes of
 Relevance to Molybdoenzymes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7573
_journal_page_last               7575
_journal_paper_doi               10.1021/ic048775m
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C24 H25 Cl Mo N4 O3'
_chemical_formula_weight         548.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.1710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7589(6)
_cell_length_b                   15.5178(10)
_cell_length_c                   15.4080(9)
_cell_measurement_reflns_used    5408
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.47
_cell_volume                     2327.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16668
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0464P)²+1.8860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                4935
_reflns_number_total             5482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048775msi20040901_095212.cif
_cod_data_source_block           sdsu5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4312045
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Mo1 Mo 0.71897(2) 0.294603(15) 0.994349(12) 0.02843(8) Uani 1 1 d . . .
Cl1 Cl 0.81323(8) 0.15979(5) 1.04263(4) 0.04356(18) Uani 1 1 d . . .
O1 O 0.62639(18) 0.37297(11) 0.91519(10) 0.0288(4) Uani 1 1 d . . .
O2 O 0.6290(2) 0.31030(14) 1.08317(11) 0.0394(5) Uani 1 1 d . . .
O3 O 0.87047(19) 0.34937(14) 1.01601(12) 0.0390(4) Uani 1 1 d . . .
N1 N 0.7003(2) 0.25174(14) 0.78741(12) 0.0259(4) Uani 1 1 d . . .
N2 N 0.7905(2) 0.24912(14) 0.85971(12) 0.0277(4) Uani 1 1 d . . .
N3 N 0.4945(2) 0.21362(13) 0.85061(12) 0.0251(4) Uani 1 1 d . . .
N4 N 0.5379(2) 0.20781(14) 0.93707(12) 0.0278(4) Uani 1 1 d . . .
C1 C 0.5504(2) 0.36944(15) 0.83449(14) 0.0247(5) Uani 1 1 d . . .
C2 C 0.5588(2) 0.27645(16) 0.79710(15) 0.0246(5) Uani 1 1 d . . .
C3 C 0.6892(4) 0.2281(3) 0.62629(18) 0.0440(7) Uani 1 1 d . . .
C4 C 0.7628(3) 0.23109(18) 0.71417(16) 0.0322(5) Uani 1 1 d . . .
C5 C 0.8975(3) 0.21525(19) 0.74073(18) 0.0359(6) Uani 1 1 d . . .
C6 C 0.9112(3) 0.22616(18) 0.83090(17) 0.0319(5) Uani 1 1 d . . .
C7 C 1.0367(3) 0.2150(3) 0.8906(2) 0.0441(7) Uani 1 1 d . . .
C8 C 0.3256(3) 0.1484(2) 0.73956(19) 0.0373(6) Uani 1 1 d . . .
C9 C 0.3938(2) 0.15605(16) 0.82845(16) 0.0283(5) Uani 1 1 d . . .
C10 C 0.3705(3) 0.11212(18) 0.90334(18) 0.0330(5) Uani 1 1 d . . .
C11 C 0.4608(3) 0.14640(17) 0.96922(16) 0.0312(5) Uani 1 1 d . . .
C12 C 0.4746(4) 0.1210(3) 1.0630(2) 0.0439(7) Uani 1 1 d . . .
C13 C 0.4007(2) 0.39269(16) 0.84821(15) 0.0268(5) Uani 1 1 d . . .
C14 C 0.3698(3) 0.42648(19) 0.92812(18) 0.0354(6) Uani 1 1 d . . .
C15 C 0.2359(3) 0.4495(2) 0.9422(2) 0.0428(7) Uani 1 1 d . . .
C16 C 0.1319(3) 0.4385(2) 0.8788(2) 0.0439(7) Uani 1 1 d . . .
C17 C 0.1611(3) 0.4045(2) 0.7997(2) 0.0414(7) Uani 1 1 d . . .
C18 C 0.2942(3) 0.38113(18) 0.78424(18) 0.0331(5) Uani 1 1 d . . .
C19 C 0.6194(2) 0.43046(16) 0.77203(15) 0.0279(5) Uani 1 1 d . . .
C20 C 0.5598(3) 0.4495(2) 0.68982(18) 0.0409(7) Uani 1 1 d . . .
C21 C 0.6289(4) 0.5008(2) 0.6332(2) 0.0455(7) Uani 1 1 d . . .
C22 C 0.7553(3) 0.53357(18) 0.6571(2) 0.0400(6) Uani 1 1 d . . .
C23 C 0.8156(3) 0.5152(2) 0.7385(2) 0.0424(7) Uani 1 1 d . . .
C24 C 0.7478(3) 0.46413(19) 0.79561(19) 0.0362(6) Uani 1 1 d . . .
H2 H 0.516(3) 0.2744(16) 0.7447(17) 0.017(6) Uiso 1 1 d . . .
H3A H 0.649(4) 0.280(3) 0.610(3) 0.056(11) Uiso 1 1 d . . .
H3B H 0.634(5) 0.185(3) 0.622(3) 0.062(12) Uiso 1 1 d . . .
H3C H 0.741(4) 0.214(2) 0.584(3) 0.065(12) Uiso 1 1 d . . .
H5 H 0.959(4) 0.195(2) 0.704(2) 0.057(11) Uiso 1 1 d . . .
H7A H 1.103(5) 0.227(3) 0.863(3) 0.074(13) Uiso 1 1 d . . .
H7B H 1.043(4) 0.161(3) 0.913(3) 0.067(12) Uiso 1 1 d . . .
H7C H 1.041(4) 0.248(3) 0.936(3) 0.061(12) Uiso 1 1 d . . .
H8A H 0.284(4) 0.201(3) 0.729(3) 0.060(11) Uiso 1 1 d . . .
H8B H 0.268(4) 0.104(2) 0.738(2) 0.043(9) Uiso 1 1 d . . .
H8C H 0.387(4) 0.145(2) 0.697(2) 0.044(9) Uiso 1 1 d . . .
H10 H 0.300(3) 0.0646(19) 0.9085(18) 0.030(7) Uiso 1 1 d . . .
H12A H 0.509(5) 0.163(3) 1.096(3) 0.081(15) Uiso 1 1 d . . .
H12B H 0.389(5) 0.109(3) 1.076(3) 0.086(15) Uiso 1 1 d . . .
H12C H 0.534(5) 0.080(3) 1.071(3) 0.071(13) Uiso 1 1 d . . .
H14 H 0.436(3) 0.4336(19) 0.970(2) 0.036(8) Uiso 1 1 d . . .
H15 H 0.215(3) 0.464(2) 0.991(2) 0.050(10) Uiso 1 1 d . . .
H16 H 0.041(4) 0.452(2) 0.892(2) 0.052(10) Uiso 1 1 d . . .
H17 H 0.098(4) 0.394(2) 0.762(2) 0.041(9) Uiso 1 1 d . . .
H18 H 0.307(3) 0.356(2) 0.735(2) 0.035(8) Uiso 1 1 d . . .
H20 H 0.468(4) 0.428(2) 0.674(2) 0.055(10) Uiso 1 1 d . . .
H21 H 0.589(4) 0.509(3) 0.581(3) 0.064(11) Uiso 1 1 d . . .
H22 H 0.796(4) 0.566(2) 0.622(2) 0.051(10) Uiso 1 1 d . . .
H23 H 0.898(4) 0.537(2) 0.756(2) 0.048(9) Uiso 1 1 d . . .
H24 H 0.787(4) 0.452(2) 0.848(2) 0.056(10) Uiso 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 0.0033 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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O2 Mo1 O3 105.13(10) . . ?
O2 Mo1 O1 100.13(9) . . ?
O3 Mo1 O1 99.80(9) . . ?
O2 Mo1 N4 88.05(9) . . ?
O3 Mo1 N4 166.67(8) . . ?
O1 Mo1 N4 79.40(7) . . ?
O2 Mo1 N2 164.08(9) . . ?
O3 Mo1 N2 90.77(8) . . ?
O1 Mo1 N2 77.49(7) . . ?
N4 Mo1 N2 76.03(7) . . ?
O2 Mo1 Cl1 94.87(7) . . ?
O3 Mo1 Cl1 93.81(7) . . ?
O1 Mo1 Cl1 156.29(5) . . ?
N4 Mo1 Cl1 82.89(5) . . ?
N2 Mo1 Cl1 83.04(5) . . ?
C1 O1 Mo1 137.68(15) . . ?
C4 N1 N2 111.6(2) . . ?
C4 N1 C2 129.5(2) . . ?
N2 N1 C2 118.98(18) . . ?
C6 N2 N1 105.52(19) . . ?
C6 N2 Mo1 134.44(17) . . ?
N1 N2 Mo1 119.70(14) . . ?
C9 N3 N4 111.67(19) . . ?
C9 N3 C2 129.6(2) . . ?
N4 N3 C2 118.7(2) . . ?
C11 N4 N3 105.4(2) . . ?
C11 N4 Mo1 134.61(17) . . ?
N3 N4 Mo1 119.98(15) . . ?
O1 C1 C13 108.43(18) . . ?
O1 C1 C19 107.67(19) . . ?
C13 C1 C19 113.9(2) . . ?
O1 C1 C2 108.99(19) . . ?
C13 C1 C2 110.18(19) . . ?
C19 C1 C2 107.53(18) . . ?
N3 C2 N1 109.62(19) . . ?
N3 C2 C1 112.08(18) . . ?
N1 C2 C1 111.0(2) . . ?
N3 C2 H2 107.6(17) . . ?
N1 C2 H2 106.5(16) . . ?
C1 C2 H2 109.8(16) . . ?
C4 C3 H3A 113(2) . . ?
C4 C3 H3B 111(3) . . ?
H3A C3 H3B 113(4) . . ?
C4 C3 H3C 115(3) . . ?
H3A C3 H3C 106(3) . . ?
H3B C3 H3C 98(3) . . ?
N1 C4 C5 105.8(2) . . ?
N1 C4 C3 123.2(2) . . ?
C5 C4 C3 131.0(2) . . ?
C4 C5 C6 107.2(2) . . ?
C4 C5 H5 123(2) . . ?
C6 C5 H5 129(2) . . ?
N2 C6 C5 109.8(2) . . ?
N2 C6 C7 122.1(2) . . ?
C5 C6 C7 128.1(3) . . ?
C6 C7 H7A 107(3) . . ?
C6 C7 H7B 112(3) . . ?
H7A C7 H7B 112(4) . . ?
C6 C7 H7C 115(3) . . ?
H7A C7 H7C 107(4) . . ?
H7B C7 H7C 105(4) . . ?
C9 C8 H8A 105(2) . . ?
C9 C8 H8B 109(2) . . ?
H8A C8 H8B 115(3) . . ?
C9 C8 H8C 112(2) . . ?
H8A C8 H8C 103(3) . . ?
H8B C8 H8C 113(3) . . ?
N3 C9 C10 106.1(2) . . ?
N3 C9 C8 123.7(2) . . ?
C10 C9 C8 130.2(3) . . ?
C9 C10 C11 106.7(2) . . ?
C9 C10 H10 125.6(16) . . ?
C11 C10 H10 127.8(16) . . ?
N4 C11 C10 110.2(2) . . ?
N4 C11 C12 122.3(3) . . ?
C10 C11 C12 127.5(3) . . ?
C11 C12 H12A 111(3) . . ?
C11 C12 H12B 105(3) . . ?
H12A C12 H12B 110(4) . . ?
C11 C12 H12C 110(3) . . ?
H12A C12 H12C 104(4) . . ?
H12B C12 H12C 116(4) . . ?
C18 C13 C14 118.5(2) . . ?
C18 C13 C1 122.8(2) . . ?
C14 C13 C1 118.7(2) . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 H14 120(2) . . ?
C13 C14 H14 120(2) . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 118(2) . . ?
C14 C15 H15 121(2) . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 119(2) . . ?
C17 C16 H16 122(2) . . ?
C16 C17 C18 120.6(3) . . ?
C16 C17 H17 120(2) . . ?
C18 C17 H17 120(2) . . ?
C17 C18 C13 120.4(3) . . ?
C17 C18 H18 117(2) . . ?
C13 C18 H18 122(2) . . ?
C24 C19 C20 118.1(2) . . ?
C24 C19 C1 119.8(2) . . ?
C20 C19 C1 121.9(2) . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20 118(2) . . ?
C21 C20 H20 121(2) . . ?
C22 C21 C20 121.1(3) . . ?
C22 C21 H21 122(3) . . ?
C20 C21 H21 117(3) . . ?
C21 C22 C23 119.2(3) . . ?
C21 C22 H22 120(2) . . ?
C23 C22 H22 121(2) . . ?
C22 C23 C24 120.3(3) . . ?
C22 C23 H23 121(2) . . ?
C24 C23 H23 119(2) . . ?
C19 C24 C23 121.0(3) . . ?
C19 C24 H24 119(2) . . ?
C23 C24 H24 120(2) . . ?
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 O2 1.6965(18) . ?
Mo1 O3 1.717(2) . ?
Mo1 O1 1.9033(17) . ?
Mo1 N4 2.343(2) . ?
Mo1 N2 2.3451(19) . ?
Mo1 Cl1 2.3825(8) . ?
O1 C1 1.402(3) . ?
N1 C4 1.360(3) . ?
N1 N2 1.369(3) . ?
N1 C2 1.451(3) . ?
N2 C6 1.337(3) . ?
N3 C9 1.353(3) . ?
N3 N4 1.371(3) . ?
N3 C2 1.449(3) . ?
N4 C11 1.332(3) . ?
C1 C13 1.534(3) . ?
C1 C19 1.539(3) . ?
C1 C2 1.558(3) . ?
C2 H2 0.88(3) . ?
C3 C4 1.487(4) . ?
C3 H3A 0.92(4) . ?
C3 H3B 0.85(4) . ?
C3 H3C 0.89(4) . ?
C4 C5 1.370(4) . ?
C5 C6 1.396(4) . ?
C5 H5 0.91(4) . ?
C6 C7 1.487(4) . ?
C7 H7A 0.83(5) . ?
C7 H7B 0.91(5) . ?
C7 H7C 0.87(4) . ?
C8 C9 1.484(4) . ?
C8 H8A 0.92(4) . ?
C8 H8B 0.89(4) . ?
C8 H8C 0.92(3) . ?
C9 C10 1.373(4) . ?
C10 C11 1.400(4) . ?
C10 H10 1.01(3) . ?
C11 C12 1.494(4) . ?
C12 H12A 0.88(5) . ?
C12 H12B 0.90(5) . ?
C12 H12C 0.87(5) . ?
C13 C18 1.391(4) . ?
C13 C14 1.391(4) . ?
C14 C15 1.387(4) . ?
C14 H14 0.88(3) . ?
C15 C16 1.366(5) . ?
C15 H15 0.82(3) . ?
C16 C17 1.376(4) . ?
C16 H16 0.94(4) . ?
C17 C18 1.386(4) . ?
C17 H17 0.83(3) . ?
C18 H18 0.88(3) . ?
C19 C24 1.382(4) . ?
C19 C20 1.387(4) . ?
C20 C21 1.390(4) . ?
C20 H20 0.97(4) . ?
C21 C22 1.361(5) . ?
C21 H21 0.88(4) . ?
C22 C23 1.376(5) . ?
C22 H22 0.86(4) . ?
C23 C24 1.388(4) . ?
C23 H23 0.90(4) . ?
C24 H24 0.89(4) . ?
