#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:04:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178547 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/54/4065419.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_4065419
loop_
_publ_author_name
'Bulak, Ece'
'Varnali, Tereza'
'Schwederski, Brigitte'
'Bubrin, Denis'
'Fiedler, Jan'
'Kaim, Wolfgang'
_publ_section_title
;
 Separation of Metal Binding and Electron Transfer Sites as a Strategy To
 Stabilize the Ligand-Reduced and Metal-Oxidized Form of [Mo(CO)4L]
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6441
_journal_paper_doi               10.1021/om2007858
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C20 H14 Cl0 Mo N6 O4'
_chemical_formula_sum            'C20 H14 Cl0 Mo N6 O4'
_chemical_formula_weight         498.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.457(5)
_cell_length_b                   16.321(6)
_cell_length_c                   17.358(7)
_cell_measurement_reflns_used    3207
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      2.22
_cell_volume                     4096(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1818
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3207
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 298
_diffrn_standards_interval_time  0
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.697
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.697
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0464
_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)+(0.0256P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                1469
_reflns_number_total             3207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2007858_si_001.cif
_cod_data_source_block           bulak01
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4065419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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
Mo Mo 0.80282(4) 0.07286(4) 0.68078(3) 0.02725(17) Uani 1 1 d .
N4 N 0.7121(4) -0.1187(3) 0.5183(3) 0.0265(15) Uani 1 1 d .
N6 N 0.7501(4) 0.1553(3) 0.4258(3) 0.0234(15) Uani 1 1 d .
N2 N 0.9463(4) 0.1129(3) 0.4579(3) 0.0249(14) Uani 1 1 d .
C16 C 0.6636(5) 0.1547(4) 0.3982(4) 0.0240(18) Uani 1 1 d .
N1 N 0.8958(4) 0.0924(3) 0.5768(3) 0.0292(15) Uani 1 1 d .
N5 N 0.6240(4) 0.0327(3) 0.4698(4) 0.0286(16) Uani 1 1 d .
C8 C 0.7393(5) -0.1708(5) 0.5767(4) 0.0326(19) Uani 1 1 d .
H8A H 0.7341 -0.2289 0.5773 0.039 Uiso 1 1 calc R
C14 C 0.5478(5) 0.2181(4) 0.3176(5) 0.0365(18) Uani 1 1 d .
H14A H 0.5306 0.2591 0.2815 0.044 Uiso 1 1 calc R
N3 N 0.7734(4) -0.0416(4) 0.6108(3) 0.0288(16) Uani 1 1 d .
C5 C 0.7744(5) 0.0952(4) 0.4735(4) 0.0253(19) Uani 1 1 d .
C6 C 0.7339(5) -0.0407(4) 0.5403(4) 0.0241(18) Uani 1 1 d .
C2 C 1.0207(5) 0.1152(5) 0.5052(4) 0.033(2) Uani 1 1 d .
H2A H 1.0831 0.1238 0.4900 0.040 Uiso 1 1 calc R
C15 C 0.6354(5) 0.2158(5) 0.3455(4) 0.039(2) Uani 1 1 d .
H15A H 0.6786 0.2561 0.3293 0.047 Uiso 1 1 calc R
C10 C 0.7114(5) 0.0312(4) 0.4945(4) 0.0202(17) Uani 1 1 d .
C11 C 0.5991(5) 0.0956(4) 0.4218(4) 0.0261(18) Uani 1 1 d .
C4 C 0.9510(5) 0.1245(5) 0.3737(4) 0.035(2) Uani 1 1 d .
H4A H 0.8887 0.1202 0.3518 0.053 Uiso 1 1 calc R
H4B H 0.9907 0.0822 0.3511 0.053 Uiso 1 1 calc R
H4C H 0.9766 0.1787 0.3623 0.053 Uiso 1 1 calc R
C7 C 0.7749(5) -0.1226(4) 0.6333(4) 0.029(2) Uani 1 1 d .
H7A H 0.7976 -0.1419 0.6813 0.035 Uiso 1 1 calc R
C1 C 0.8724(5) 0.0983(4) 0.5020(4) 0.0228(18) Uani 1 1 d .
C12 C 0.5054(5) 0.1006(5) 0.3949(4) 0.034(2) Uani 1 1 d .
H12A H 0.4600 0.0633 0.4133 0.041 Uiso 1 1 calc R
C13 C 0.4826(5) 0.1597(5) 0.3424(4) 0.041(2) Uani 1 1 d .
H13A H 0.4215 0.1614 0.3222 0.049 Uiso 1 1 calc R
C3 C 0.9898(5) 0.1028(4) 0.5783(4) 0.032(2) Uani 1 1 d .
H3A H 1.0274 0.1016 0.6232 0.038 Uiso 1 1 calc R
O72 O 0.6875(4) 0.0291(3) 0.8285(3) 0.0538(15) Uani 1 1 d .
O62 O 0.8428(4) 0.2357(3) 0.7666(3) 0.0493(17) Uani 1 1 d .
O52 O 0.6214(4) 0.1684(4) 0.6307(3) 0.0505(16) Uani 1 1 d .
C51 C 0.6864(6) 0.1289(4) 0.6433(4) 0.034(2) Uani 1 1 d .
C9 C 0.6644(6) -0.1455(4) 0.4469(4) 0.039(2) Uani 1 1 d .
H9A H 0.6520 -0.0977 0.4142 0.059 Uiso 1 1 calc R
H9B H 0.6058 -0.1721 0.4604 0.059 Uiso 1 1 calc R
H9C H 0.7038 -0.1843 0.4189 0.059 Uiso 1 1 calc R
C71 C 0.7303(5) 0.0437(4) 0.7696(4) 0.035(2) Uani 1 1 d .
C61 C 0.8288(5) 0.1755(5) 0.7340(4) 0.034(2) Uani 1 1 d .
C81 C 0.9170(6) 0.0350(5) 0.7391(5) 0.039(2) Uani 1 1 d .
O82 O 0.9832(4) 0.0273(4) 0.7764(3) 0.062(2) Uani 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
C71 Mo C61 86.4(3)
C71 Mo C51 85.2(3)
C61 Mo C51 85.7(3)
C71 Mo C81 88.2(3)
C61 Mo C81 82.5(3)
C51 Mo C81 166.7(3)
C71 Mo N3 97.1(3)
C61 Mo N3 175.9(3)
C51 Mo N3 92.5(2)
C81 Mo N3 99.7(3)
C71 Mo N1 173.3(3)
C61 Mo N1 98.2(2)
C51 Mo N1 100.0(2)
C81 Mo N1 87.6(3)
N3 Mo N1 78.5(2)
C6 N4 C8 107.6(6)
C6 N4 C9 128.0(6)
C8 N4 C9 124.3(6)
C5 N6 C16 117.6(6)
C1 N2 C2 107.1(6)
C1 N2 C4 128.8(6)
C2 N2 C4 124.1(6)
N6 C16 C11 121.4(7)
N6 C16 C15 119.7(7)
C11 C16 C15 118.8(7)
C1 N1 C3 105.0(6)
C1 N1 Mo 128.9(5)
C3 N1 Mo 126.1(5)
C10 N5 C11 117.2(6)
C7 C8 N4 106.3(7)
C15 C14 C13 119.8(7)
C6 N3 C7 105.9(6)
C6 N3 Mo 123.7(5)
C7 N3 Mo 129.4(5)
N6 C5 C10 121.9(6)
N6 C5 C1 115.3(6)
C10 C5 C1 122.8(6)
N3 C6 N4 110.0(6)
N3 C6 C10 126.8(7)
N4 C6 C10 123.2(6)
N2 C2 C3 107.5(7)
C14 C15 C16 121.4(7)
N5 C10 C5 120.5(6)
N5 C10 C6 113.7(6)
C5 C10 C6 125.8(7)
N5 C11 C16 121.3(7)
N5 C11 C12 119.2(6)
C16 C11 C12 119.6(7)
C8 C7 N3 110.2(7)
N2 C1 N1 111.4(6)
N2 C1 C5 124.9(6)
N1 C1 C5 123.5(6)
C13 C12 C11 119.0(7)
C12 C13 C14 121.2(7)
C2 C3 N1 109.0(7)
O52 C51 Mo 170.2(7)
O72 C71 Mo 175.8(6)
O62 C61 Mo 178.6(6)
O82 C81 Mo 168.3(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo C71 1.924(8)
Mo C61 1.949(9)
Mo C51 2.022(9)
Mo C81 2.032(10)
Mo N3 2.269(6)
Mo N1 2.273(6)
N4 C6 1.365(8)
N4 C8 1.381(8)
N4 C9 1.484(9)
N6 C5 1.332(8)
N6 C16 1.339(8)
N2 C1 1.335(8)
N2 C2 1.353(9)
N2 C4 1.475(8)
C16 C11 1.403(9)
C16 C15 1.413(10)
N1 C1 1.345(8)
N1 C3 1.371(8)
N5 C10 1.335(9)
N5 C11 1.370(8)
C8 C7 1.360(10)
C14 C15 1.356(9)
C14 C13 1.409(10)
N3 C6 1.350(8)
N3 C7 1.377(8)
C5 C10 1.432(9)
C5 C1 1.502(9)
C6 C10 1.456(9)
C2 C3 1.360(10)
C11 C12 1.435(9)
C12 C13 1.369(10)
O72 C71 1.220(8)
O62 C61 1.152(8)
O52 C51 1.161(9)
C81 O82 1.162(9)
