#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:52:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179159 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/20/4312046.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_4312046
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            'C30 H39 Cl2 Mo N6 O4'
_chemical_formula_weight         714.51
_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                72.0210(10)
_cell_angle_beta                 73.2200(10)
_cell_angle_gamma                80.7560(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7513(6)
_cell_length_b                   13.6366(9)
_cell_length_c                   14.8639(10)
_cell_measurement_reflns_used    8606
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.44
_cell_volume                     1610.38(19)
_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 0.918
_diffrn_measured_fraction_theta_max 0.918
_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  0.0239
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11908
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue/Purple
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.845
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0805
_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)+(0.0723P)²+7.2001P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.1968
_reflns_number_gt                6762
_reflns_number_total             7285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048775msi20040901_095225.cif
_cod_data_source_block           sdsu8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4312046
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
Mo1 Mo 0.60605(5) 0.89056(3) 0.26657(4) 0.03853(16) Uani 1 1 d . . .
Cl1 Cl 0.49834(18) 0.99028(12) 0.13850(11) 0.0504(3) Uani 1 1 d . . .
Cl2 Cl 0.36585(18) 0.83172(13) 0.36468(13) 0.0578(4) Uani 1 1 d . . .
O1 O 0.6564(4) 0.7703(2) 0.2172(2) 0.0298(7) Uani 1 1 d . . .
O2 O 0.6022(5) 1.0070(4) 0.3199(3) 0.0569(13) Uani 1 1 d . . .
N1 N 0.9676(4) 0.8335(3) 0.1761(3) 0.0272(7) Uani 1 1 d . . .
N2 N 0.8554(4) 0.9166(3) 0.1782(3) 0.0286(8) Uani 1 1 d . . .
N3 N 0.8736(4) 0.7285(3) 0.3374(3) 0.0294(8) Uani 1 1 d . . .
N4 N 0.7395(4) 0.7882(3) 0.3706(3) 0.0300(8) Uani 1 1 d . . .
C1 C 0.9232(5) 0.7308(3) 0.2344(3) 0.0260(8) Uani 1 1 d . . .
H1A H 1.0181 0.6812 0.2242 0.031 Uiso 1 1 calc R . .
C2 C 0.7860(5) 0.6978(3) 0.2045(3) 0.0253(8) Uani 1 1 d . . .
C3 C 0.8374(5) 0.6974(3) 0.0971(3) 0.0275(9) Uani 1 1 d . . .
C4 C 0.9708(6) 0.6371(4) 0.0594(4) 0.0354(10) Uani 1 1 d . . .
H4A H 1.0377 0.5986 0.0996 0.042 Uiso 1 1 calc R . .
C5 C 1.0053(7) 0.6335(4) -0.0360(4) 0.0417(12) Uani 1 1 d . . .
H5A H 1.0951 0.5921 -0.0599 0.050 Uiso 1 1 calc R . .
C6 C 0.9103(7) 0.6896(4) -0.0968(4) 0.0430(12) Uani 1 1 d . . .
H6A H 0.9341 0.6861 -0.1616 0.052 Uiso 1 1 calc R . .
C7 C 0.7796(7) 0.7511(4) -0.0613(4) 0.0424(12) Uani 1 1 d . . .
H7A H 0.7148 0.7904 -0.1024 0.051 Uiso 1 1 calc R . .
C8 C 0.7433(6) 0.7553(4) 0.0348(4) 0.0346(10) Uani 1 1 d . . .
H8A H 0.6543 0.7977 0.0580 0.041 Uiso 1 1 calc R . .
C9 C 0.7388(5) 0.5913(3) 0.2730(3) 0.0286(9) Uani 1 1 d . . .
C10 C 0.8525(6) 0.5078(4) 0.2875(4) 0.0380(11) Uani 1 1 d . . .
H10A H 0.9608 0.5160 0.2544 0.046 Uiso 1 1 calc R . .
C11 C 0.8064(7) 0.4126(4) 0.3507(5) 0.0484(14) Uani 1 1 d . . .
H11A H 0.8838 0.3568 0.3610 0.058 Uiso 1 1 calc R . .
C12 C 0.6477(8) 0.3997(5) 0.3984(5) 0.0550(16) Uani 1 1 d . . .
H12A H 0.6167 0.3355 0.4418 0.066 Uiso 1 1 calc R . .
C13 C 0.5344(8) 0.4814(5) 0.3824(5) 0.0584(17) Uani 1 1 d . . .
H13A H 0.4257 0.4722 0.4137 0.070 Uiso 1 1 calc R . .
C14 C 0.5794(6) 0.5771(4) 0.3204(4) 0.0438(12) Uani 1 1 d . . .
H14A H 0.5014 0.6326 0.3105 0.053 Uiso 1 1 calc R . .
C15 C 1.2637(6) 0.7942(4) 0.1180(4) 0.0434(12) Uani 1 1 d . . .
H15A H 1.2354 0.7234 0.1490 0.065 Uiso 1 1 calc R . .
H15B H 1.3375 0.8095 0.1487 0.065 Uiso 1 1 calc R . .
H15C H 1.3142 0.8027 0.0490 0.065 Uiso 1 1 calc R . .
C16 C 1.1163(5) 0.8661(4) 0.1293(4) 0.0332(10) Uani 1 1 d . . .
C17 C 1.0981(6) 0.9717(4) 0.0978(4) 0.0390(11) Uani 1 1 d . . .
H17A H 1.1797 1.0162 0.0615 0.047 Uiso 1 1 calc R . .
C18 C 0.9370(6) 1.0009(4) 0.1294(4) 0.0330(10) Uani 1 1 d . . .
C19 C 0.8563(7) 1.1065(4) 0.1171(5) 0.0452(13) Uani 1 1 d . . .
H19A H 0.7425 1.1023 0.1472 0.068 Uiso 1 1 calc R . .
H19B H 0.8733 1.1421 0.0480 0.068 Uiso 1 1 calc R . .
H19C H 0.9004 1.1443 0.1482 0.068 Uiso 1 1 calc R . .
C20 C 1.0997(7) 0.6128(5) 0.3949(4) 0.0444(12) Uani 1 1 d . . .
H20A H 1.1337 0.6095 0.3277 0.067 Uiso 1 1 calc R . .
H20B H 1.0836 0.5437 0.4385 0.067 Uiso 1 1 calc R . .
H20C H 1.1813 0.6420 0.4089 0.067 Uiso 1 1 calc R . .
C21 C 0.9472(6) 0.6789(4) 0.4096(4) 0.0338(10) Uani 1 1 d . . .
C22 C 0.8557(6) 0.7058(4) 0.4918(4) 0.0400(11) Uani 1 1 d . . .
H22A H 0.8746 0.6825 0.5544 0.048 Uiso 1 1 calc R . .
C23 C 0.7293(6) 0.7740(4) 0.4649(4) 0.0353(10) Uani 1 1 d . . .
C24 C 0.6027(7) 0.8299(5) 0.5268(4) 0.0487(14) Uani 1 1 d . . .
H24A H 0.5301 0.8718 0.4887 0.073 Uiso 1 1 calc R . .
H24B H 0.6520 0.8740 0.5487 0.073 Uiso 1 1 calc R . .
H24C H 0.5435 0.7801 0.5830 0.073 Uiso 1 1 calc R . .
O1S O 0.2450(5) 0.5331(4) 0.1897(4) 0.0592(11) Uani 1 1 d . . .
N1S N 0.4677(5) 0.4263(3) 0.1589(4) 0.0417(10) Uani 1 1 d . . .
C1S C 0.3130(6) 0.4469(5) 0.1986(4) 0.0426(12) Uani 1 1 d . . .
C2S C 0.5412(9) 0.3209(5) 0.1749(6) 0.0650(18) Uani 1 1 d . . .
H2SA H 0.4603 0.2730 0.2138 0.097 Uiso 1 1 calc R . .
H2SB H 0.6234 0.3130 0.2092 0.097 Uiso 1 1 calc R . .
H2SC H 0.5890 0.3063 0.1124 0.097 Uiso 1 1 calc R . .
C3S C 0.5696(7) 0.5099(5) 0.1024(6) 0.0604(17) Uani 1 1 d . . .
H3SA H 0.5057 0.5755 0.0968 0.091 Uiso 1 1 calc R . .
H3SB H 0.6196 0.5014 0.0376 0.091 Uiso 1 1 calc R . .
H3SC H 0.6518 0.5086 0.1348 0.091 Uiso 1 1 calc R . .
O2S O 0.8514(6) 0.7893(3) -0.3204(3) 0.0570(11) Uani 1 1 d . . .
N2S N 0.9943(6) 0.9274(4) -0.3601(4) 0.0442(10) Uani 1 1 d . . .
C4S C 0.8616(7) 0.8790(5) -0.3247(5) 0.0473(13) Uani 1 1 d . . .
C5S C 1.1441(9) 0.8761(7) -0.4016(7) 0.079(2) Uani 1 1 d . . .
H5SA H 1.1276 0.8056 -0.3960 0.119 Uiso 1 1 calc R . .
H5SB H 1.2224 0.8755 -0.3666 0.119 Uiso 1 1 calc R . .
H5SC H 1.1828 0.9128 -0.4700 0.119 Uiso 1 1 calc R . .
C6S C 1.0013(9) 1.0332(5) -0.3639(6) 0.0638(18) Uani 1 1 d . . .
H6SA H 0.8958 1.0611 -0.3349 0.096 Uiso 1 1 calc R . .
H6SB H 1.0368 1.0734 -0.4315 0.096 Uiso 1 1 calc R . .
H6SC H 1.0759 1.0367 -0.3280 0.096 Uiso 1 1 calc R . .
H1SA H 0.260(9) 0.392(6) 0.235(5) 0.06(2) Uiso 1 1 d . . .
H1SB H 0.782(9) 0.925(6) -0.306(5) 0.06(2) 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'
Cl Cl 0.1484 0.1585 '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'
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 Mo1 O2 167.70(16) . . ?
O1 Mo1 N4 79.96(14) . . ?
O2 Mo1 N4 90.76(16) . . ?
O1 Mo1 N2 79.96(13) . . ?
O2 Mo1 N2 90.52(15) . . ?
N4 Mo1 N2 79.86(14) . . ?
O1 Mo1 Cl2 91.41(10) . . ?
O2 Mo1 Cl2 97.08(12) . . ?
N4 Mo1 Cl2 92.45(11) . . ?
N2 Mo1 Cl2 169.28(10) . . ?
O1 Mo1 Cl1 93.71(10) . . ?
O2 Mo1 Cl1 94.53(13) . . ?
N4 Mo1 Cl1 170.99(11) . . ?
N2 Mo1 Cl1 92.80(11) . . ?
Cl2 Mo1 Cl1 94.12(6) . . ?
C2 O1 Mo1 136.4(3) . . ?
C16 N1 N2 110.6(4) . . ?
C16 N1 C1 128.6(4) . . ?
N2 N1 C1 119.7(3) . . ?
C18 N2 N1 105.6(4) . . ?
C18 N2 Mo1 134.5(3) . . ?
N1 N2 Mo1 119.5(3) . . ?
C21 N3 N4 111.1(4) . . ?
C21 N3 C1 129.2(4) . . ?
N4 N3 C1 119.5(4) . . ?
C23 N4 N3 105.8(4) . . ?
C23 N4 Mo1 134.2(3) . . ?
N3 N4 Mo1 119.8(3) . . ?
N1 C1 N3 109.0(4) . . ?
N1 C1 C2 111.5(3) . . ?
N3 C1 C2 110.4(3) . . ?
O1 C2 C3 108.8(3) . . ?
O1 C2 C9 109.3(3) . . ?
C3 C2 C9 111.8(3) . . ?
O1 C2 C1 107.2(3) . . ?
C3 C2 C1 111.0(3) . . ?
C9 C2 C1 108.5(3) . . ?
C8 C3 C4 118.1(4) . . ?
C8 C3 C2 119.0(4) . . ?
C4 C3 C2 122.8(4) . . ?
C5 C4 C3 120.6(5) . . ?
C4 C5 C6 121.0(5) . . ?
C5 C6 C7 119.1(5) . . ?
C6 C7 C8 120.5(5) . . ?
C7 C8 C3 120.7(5) . . ?
C14 C9 C10 119.1(4) . . ?
C14 C9 C2 119.4(4) . . ?
C10 C9 C2 121.5(4) . . ?
C11 C10 C9 120.2(5) . . ?
C12 C11 C10 120.2(5) . . ?
C13 C12 C11 119.7(5) . . ?
C12 C13 C14 120.5(5) . . ?
C9 C14 C13 120.3(5) . . ?
N1 C16 C17 106.6(4) . . ?
N1 C16 C15 123.3(4) . . ?
C17 C16 C15 130.2(4) . . ?
C16 C17 C18 107.3(4) . . ?
N2 C18 C17 109.9(4) . . ?
N2 C18 C19 121.5(4) . . ?
C17 C18 C19 128.5(4) . . ?
N3 C21 C22 106.1(4) . . ?
N3 C21 C20 123.7(5) . . ?
C22 C21 C20 130.2(5) . . ?
C21 C22 C23 107.1(4) . . ?
N4 C23 C22 109.8(4) . . ?
N4 C23 C24 122.4(5) . . ?
C22 C23 C24 127.7(5) . . ?
C1S N1S C3S 120.3(5) . . ?
C1S N1S C2S 121.6(5) . . ?
C3S N1S C2S 118.0(5) . . ?
O1S C1S N1S 125.0(6) . . ?
C4S N2S C6S 123.8(6) . . ?
C4S N2S C5S 120.8(6) . . ?
C6S N2S C5S 115.4(6) . . ?
O2S C4S N2S 125.5(6) . . ?
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 O1 1.935(3) . ?
Mo1 O2 1.974(5) . ?
Mo1 N4 2.211(4) . ?
Mo1 N2 2.219(4) . ?
Mo1 Cl2 2.2888(16) . ?
Mo1 Cl1 2.3212(15) . ?
O1 C2 1.390(5) . ?
N1 C16 1.359(6) . ?
N1 N2 1.377(5) . ?
N1 C1 1.448(5) . ?
N2 C18 1.344(6) . ?
N3 C21 1.354(6) . ?
N3 N4 1.375(5) . ?
N3 C1 1.458(6) . ?
N4 C23 1.333(6) . ?
C1 C2 1.564(6) . ?
C2 C3 1.529(6) . ?
C2 C9 1.535(6) . ?
C3 C8 1.393(6) . ?
C3 C4 1.397(6) . ?
C4 C5 1.376(7) . ?
C5 C6 1.378(8) . ?
C6 C7 1.381(8) . ?
C7 C8 1.387(7) . ?
C9 C14 1.384(7) . ?
C9 C10 1.393(7) . ?
C10 C11 1.388(7) . ?
C11 C12 1.377(9) . ?
C12 C13 1.378(9) . ?
C13 C14 1.385(8) . ?
C15 C16 1.492(7) . ?
C16 C17 1.368(7) . ?
C17 C18 1.385(7) . ?
C18 C19 1.481(7) . ?
C20 C21 1.486(7) . ?
C21 C22 1.373(7) . ?
C22 C23 1.394(7) . ?
C23 C24 1.492(7) . ?
O1S C1S 1.216(7) . ?
N1S C1S 1.334(7) . ?
N1S C3S 1.450(7) . ?
N1S C2S 1.455(8) . ?
O2S C4S 1.222(8) . ?
N2S C4S 1.319(8) . ?
N2S C6S 1.437(8) . ?
N2S C5S 1.447(8) . ?
