#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/89/1518955.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_1518955
loop_
_publ_author_name
'Tsurugi, Hayato'
'Hayakawa, Akio'
'Kando, Shun'
'Sugino, Yoshitaka'
'Mashima, Kazushi'
_publ_section_title
;
 Mixed-ligand complexes of paddlewheel dinuclear molybdenum as
 hydrodehalogenation catalysts for polyhaloalkanes
;
_journal_issue                   6
_journal_name_full               'Chem. Sci.'
_journal_page_first              3434
_journal_paper_doi               10.1039/C5SC00721F
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C34 H36 Cl4 Mo2 N6 O4'
_chemical_formula_sum            'C34 H36 Cl4 Mo2 N6 O4'
_chemical_formula_weight         926.39
_chemical_name_common            11a
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_update_record
;
2015-01-31 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.276(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.752(5)
_cell_length_b                   15.014(7)
_cell_length_c                   11.140(5)
_cell_measurement_reflns_used    4120
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      6.25
_cell_volume                     1855.4(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17056
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         5.98
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.8799
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.566
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0571
_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)+(0.0342P)²+4.3628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                3888
_reflns_number_total             4159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc00721f1.cif
_cod_data_source_block           shelxl-11a
_cod_depositor_comments
'Adding full bibliography for 1518952--1518955.cif.'
_cod_database_code               1518955
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
Mo1 Mo 0.01930(3) 0.43747(2) 0.08493(3) 0.02171(12) Uani 1 1 d .
Cl1 Cl 0.10219(9) 0.41627(7) 0.31241(10) 0.0301(2) Uani 1 1 d .
Cl2 Cl -0.07875(9) 0.41023(6) -0.13976(9) 0.0258(2) Uani 1 1 d .
O1 O 0.4784(3) 0.1208(2) 0.2414(3) 0.0405(8) Uani 1 1 d .
O2 O -0.3154(3) 0.3228(2) 0.4759(3) 0.0366(7) Uani 1 1 d .
N1 N 0.1848(3) 0.4167(2) 0.0531(3) 0.0240(7) Uani 1 1 d .
N2 N -0.1532(3) 0.4694(2) 0.0991(3) 0.0231(7) Uani 1 1 d .
N3 N 0.0007(3) 0.2926(2) 0.0824(3) 0.0232(7) Uani 1 1 d .
C1 C 0.2176(4) 0.4642(3) -0.0301(4) 0.0249(8) Uani 1 1 d .
H1 H 0.2922 0.4500 -0.0413 0.030 Uiso 1 1 calc R
C2 C 0.2628(3) 0.3422(3) 0.1053(4) 0.0243(8) Uani 1 1 d .
C3 C 0.3357(4) 0.3410(3) 0.2307(4) 0.0326(9) Uani 1 1 d .
H3 H 0.3356 0.3902 0.2842 0.039 Uiso 1 1 calc R
C4 C 0.4102(4) 0.2676(3) 0.2799(4) 0.0357(10) Uani 1 1 d .
H4 H 0.4611 0.2675 0.3662 0.043 Uiso 1 1 calc R
C5 C 0.4095(4) 0.1961(3) 0.2035(4) 0.0315(9) Uani 1 1 d .
C6 C 0.3363(4) 0.1970(3) 0.0766(4) 0.0333(10) Uani 1 1 d .
H6 H 0.3363 0.1476 0.0232 0.040 Uiso 1 1 calc R
C7 C 0.2632(4) 0.2700(3) 0.0279(4) 0.0295(9) Uani 1 1 d .
H7 H 0.2132 0.2705 -0.0588 0.035 Uiso 1 1 calc R
C8 C 0.5444(5) 0.1118(4) 0.3734(5) 0.0506(14) Uani 1 1 d .
H8A H 0.4881 0.1061 0.4212 0.061 Uiso 1 1 calc R
H8B H 0.5953 0.1645 0.4030 0.061 Uiso 1 1 calc R
H8C H 0.5954 0.0585 0.3869 0.061 Uiso 1 1 calc R
C9 C -0.2019(3) 0.4333(3) 0.1916(4) 0.0236(8) Uani 1 1 d .
C10 C -0.2033(4) 0.3414(3) 0.2107(4) 0.0287(9) Uani 1 1 d .
H10 H -0.1761 0.3024 0.1588 0.034 Uiso 1 1 calc R
C11 C -0.2438(4) 0.3066(3) 0.3042(4) 0.0311(9) Uani 1 1 d .
H11 H -0.2435 0.2440 0.3167 0.037 Uiso 1 1 calc R
C12 C -0.2850(4) 0.3632(3) 0.3801(4) 0.0303(9) Uani 1 1 d .
C13 C -0.2902(4) 0.4536(3) 0.3577(4) 0.0315(9) Uani 1 1 d .
H13 H -0.3223 0.4922 0.4060 0.038 Uiso 1 1 calc R
C14 C -0.2485(4) 0.4879(3) 0.2642(4) 0.0299(9) Uani 1 1 d .
H14 H -0.2520 0.5504 0.2497 0.036 Uiso 1 1 calc R
C15 C -0.3589(5) 0.3790(4) 0.5539(5) 0.0441(12) Uani 1 1 d .
H15A H -0.3822 0.3427 0.6151 0.053 Uiso 1 1 calc R
H15B H -0.4292 0.4123 0.5006 0.053 Uiso 1 1 calc R
H15C H -0.2954 0.4208 0.5998 0.053 Uiso 1 1 calc R
C16 C 0.0019(4) 0.2188(3) 0.0780(4) 0.0301(9) Uani 1 1 d .
C17 C 0.0045(4) 0.1208(3) 0.0745(5) 0.0380(11) Uani 1 1 d .
H17A H -0.0446 0.1000 -0.0101 0.046 Uiso 1 1 calc R
H17B H -0.0279 0.0967 0.1383 0.046 Uiso 1 1 calc R
H17C H 0.0878 0.1005 0.0930 0.046 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 0.0033 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'
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'
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'
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
N1 Mo1 N2 173.28(12) . .
N1 Mo1 N3 86.81(12) . .
N2 Mo1 N3 97.53(12) . .
N1 Mo1 Cl2 88.67(9) . 3_565
N2 Mo1 Cl2 88.34(9) . 3_565
N3 Mo1 Cl2 165.25(9) . 3_565
N1 Mo1 Cl1 94.69(10) . .
N2 Mo1 Cl1 90.91(9) . .
N3 Mo1 Cl1 83.48(9) . .
Cl2 Mo1 Cl1 82.90(4) 3_565 .
N1 Mo1 Cl2 87.24(10) . .
N2 Mo1 Cl2 88.57(9) . .
N3 Mo1 Cl2 78.87(9) . .
Cl2 Mo1 Cl2 114.94(3) 3_565 .
Cl1 Mo1 Cl2 162.12(4) . .
N1 Mo1 Mo1 86.19(9) . 3_565
N2 Mo1 Mo1 87.13(9) . 3_565
N3 Mo1 Mo1 135.84(9) . 3_565
Cl2 Mo1 Mo1 57.66(4) 3_565 3_565
Cl1 Mo1 Mo1 140.54(3) . 3_565
Cl2 Mo1 Mo1 57.28(3) . 3_565
Mo1 Cl2 Mo1 65.06(3) 3_565 .
C5 O1 C8 117.5(4) . .
C12 O2 C15 116.8(4) . .
C1 N1 C2 114.0(3) . .
C1 N1 Mo1 122.4(3) . .
C2 N1 Mo1 123.0(3) . .
C1 N2 C9 114.2(3) 3_565 .
C1 N2 Mo1 119.8(3) 3_565 .
C9 N2 Mo1 125.4(2) . .
C16 N3 Mo1 172.8(3) . .
N1 C1 N2 124.4(4) . 3_565
N1 C1 H1 117.8 . .
N2 C1 H1 117.8 3_565 .
C3 C2 C7 119.5(4) . .
C3 C2 N1 121.3(4) . .
C7 C2 N1 119.2(4) . .
C2 C3 C4 120.4(4) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C5 C4 C3 119.9(4) . .
C5 C4 H4 120.0 . .
C3 C4 H4 120.0 . .
C4 C5 O1 124.9(4) . .
C4 C5 C6 119.9(4) . .
O1 C5 C6 115.1(4) . .
C7 C6 C5 120.0(4) . .
C7 C6 H6 120.0 . .
C5 C6 H6 120.0 . .
C2 C7 C6 120.2(4) . .
C2 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
O1 C8 H8A 109.5 . .
O1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
O1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C14 C9 C10 118.0(4) . .
C14 C9 N2 121.4(3) . .
C10 C9 N2 120.6(4) . .
C11 C10 C9 120.8(4) . .
C11 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
C10 C11 C12 120.1(4) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
O2 C12 C13 124.6(4) . .
O2 C12 C11 115.8(4) . .
C13 C12 C11 119.6(4) . .
C12 C13 C14 119.8(4) . .
C12 C13 H13 120.1 . .
C14 C13 H13 120.1 . .
C9 C14 C13 121.5(4) . .
C9 C14 H14 119.2 . .
C13 C14 H14 119.2 . .
O2 C15 H15A 109.5 . .
O2 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
O2 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N3 C16 C17 179.0(5) . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 N1 2.112(3) .
Mo1 N2 2.139(3) .
Mo1 N3 2.186(3) .
Mo1 Cl2 2.4099(13) 3_565
Mo1 Cl1 2.4171(15) .
Mo1 Cl2 2.4200(14) .
Mo1 Mo1 2.5972(10) 3_565
Cl2 Mo1 2.4100(14) 3_565
O1 C5 1.372(5) .
O1 C8 1.425(6) .
O2 C12 1.373(5) .
O2 C15 1.422(6) .
N1 C1 1.325(5) .
N1 C2 1.442(5) .
N2 C1 1.332(5) 3_565
N2 C9 1.440(5) .
N3 C16 1.109(5) .
C1 N2 1.332(5) 3_565
C1 H1 0.9500 .
C2 C3 1.377(6) .
C2 C7 1.386(6) .
C3 C4 1.401(6) .
C3 H3 0.9500 .
C4 C5 1.369(6) .
C4 H4 0.9500 .
C5 C6 1.392(6) .
C6 C7 1.388(6) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C14 1.386(6) .
C9 C10 1.396(6) .
C10 C11 1.382(6) .
C10 H10 0.9500 .
C11 C12 1.393(6) .
C11 H11 0.9500 .
C12 C13 1.378(6) .
C13 C14 1.388(6) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.472(6) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Mo1 Cl2 Mo1 -87.24(9) . 3_565
N2 Mo1 Cl2 Mo1 87.51(9) . 3_565
N3 Mo1 Cl2 Mo1 -174.53(9) . 3_565
Cl2 Mo1 Cl2 Mo1 0.0 3_565 3_565
Cl1 Mo1 Cl2 Mo1 176.03(11) . 3_565
N2 Mo1 N1 C1 5.7(12) . .
N3 Mo1 N1 C1 136.1(3) . .
Cl2 Mo1 N1 C1 -57.9(3) 3_565 .
Cl1 Mo1 N1 C1 -140.7(3) . .
Cl2 Mo1 N1 C1 57.1(3) . .
Mo1 Mo1 N1 C1 -0.3(3) 3_565 .
N2 Mo1 N1 C2 -165.0(9) . .
N3 Mo1 N1 C2 -34.6(3) . .
Cl2 Mo1 N1 C2 131.4(3) 3_565 .
Cl1 Mo1 N1 C2 48.6(3) . .
Cl2 Mo1 N1 C2 -113.6(3) . .
Mo1 Mo1 N1 C2 -170.9(3) 3_565 .
N1 Mo1 N2 C1 -7.8(12) . 3_565
N3 Mo1 N2 C1 -137.8(3) . 3_565
Cl2 Mo1 N2 C1 55.8(3) 3_565 3_565
Cl1 Mo1 N2 C1 138.7(3) . 3_565
Cl2 Mo1 N2 C1 -59.2(3) . 3_565
Mo1 Mo1 N2 C1 -1.9(3) 3_565 3_565
N1 Mo1 N2 C9 -178.5(9) . .
N3 Mo1 N2 C9 51.5(3) . .
Cl2 Mo1 N2 C9 -114.9(3) 3_565 .
Cl1 Mo1 N2 C9 -32.0(3) . .
Cl2 Mo1 N2 C9 130.1(3) . .
Mo1 Mo1 N2 C9 -172.6(3) 3_565 .
N1 Mo1 N3 C16 -5(3) . .
N2 Mo1 N3 C16 170(3) . .
Cl2 Mo1 N3 C16 -77(3) 3_565 .
Cl1 Mo1 N3 C16 -100(3) . .
Cl2 Mo1 N3 C16 83(3) . .
Mo1 Mo1 N3 C16 77(3) 3_565 .
C2 N1 C1 N2 173.3(4) . 3_565
Mo1 N1 C1 N2 1.9(5) . 3_565
C1 N1 C2 C3 110.9(4) . .
Mo1 N1 C2 C3 -77.8(4) . .
C1 N1 C2 C7 -69.9(5) . .
Mo1 N1 C2 C7 101.5(4) . .
C7 C2 C3 C4 0.2(6) . .
N1 C2 C3 C4 179.5(4) . .
C2 C3 C4 C5 -0.8(7) . .
C3 C4 C5 O1 -180.0(4) . .
C3 C4 C5 C6 1.0(7) . .
C8 O1 C5 C4 8.0(6) . .
C8 O1 C5 C6 -172.9(4) . .
C4 C5 C6 C7 -0.6(7) . .
O1 C5 C6 C7 -179.7(4) . .
C3 C2 C7 C6 0.2(6) . .
N1 C2 C7 C6 -179.1(4) . .
C5 C6 C7 C2 0.0(7) . .
C1 N2 C9 C14 -41.9(5) 3_565 .
Mo1 N2 C9 C14 129.3(3) . .
C1 N2 C9 C10 138.2(4) 3_565 .
Mo1 N2 C9 C10 -50.6(5) . .
C14 C9 C10 C11 -3.5(6) . .
N2 C9 C10 C11 176.4(4) . .
C9 C10 C11 C12 0.6(6) . .
C15 O2 C12 C13 2.1(6) . .
C15 O2 C12 C11 -179.3(4) . .
C10 C11 C12 O2 -175.7(4) . .
C10 C11 C12 C13 3.0(6) . .
O2 C12 C13 C14 175.1(4) . .
C11 C12 C13 C14 -3.4(6) . .
C10 C9 C14 C13 3.0(6) . .
N2 C9 C14 C13 -176.9(4) . .
C12 C13 C14 C9 0.4(6) . .
Mo1 N3 C16 C17 95(28) . .
