#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:49:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179492 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/89/4338944.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_4338944
loop_
_publ_author_name
'Cotton, F. Albert'
'Li, Zhong'
'Liu, Chun Y.'
'Murillo, Carlos A.'
_publ_section_title
;
 Enhancement in electronic communication upon replacement of Mo-O by Mo-S
 bonds in tetranuclear clusters of the type [Mo2]2(mu-E-E)2 (E = O or S).
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9294
_journal_page_last               9302
_journal_paper_doi               10.1021/ic701303k
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[Mo2(C15H15N2O2)2]2(C6H4O2)2, 0.5(CH2Cl2)'
_chemical_formula_sum            'C73 H70 Cl2 Mo4 N8 O12'
_chemical_formula_weight         1706.03
_chemical_name_common            '[Mo2(DAniF)2]2(C6H4O2)2, 0.5(CH2Cl2)'
_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                104.881(5)
_cell_angle_beta                 108.272(4)
_cell_angle_gamma                106.460(5)
_cell_formula_units_Z            1
_cell_length_a                   10.590(3)
_cell_length_b                   14.603(4)
_cell_length_c                   14.675(4)
_cell_measurement_reflns_used    7728
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.75
_cell_measurement_theta_min      2.21
_cell_volume                     1912.0(9)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'None (area detector data)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9812
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.9407
_exptl_absorpt_correction_T_min  0.7372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.559
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4961
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0581
_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)+(0.0988P)²+8.2648P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                4260
_reflns_number_total             4961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701303k.cif
_cod_data_source_block           xl
_cod_original_cell_volume        1912.2(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338944
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
Mo1 Mo 0.60181(6) 1.12636(4) 0.98651(4) 0.0225(2) Uani 1 1 d .
Mo2 Mo 0.53574(6) 1.12573(4) 1.10820(4) 0.0227(2) Uani 1 1 d .
N1 N 0.5152(6) 1.2333(4) 0.9539(4) 0.0261(13) Uani 1 1 d .
N2 N 0.4486(6) 1.2351(4) 1.0875(4) 0.0264(13) Uani 1 1 d .
N3 N 0.8094(6) 1.2388(4) 1.0906(4) 0.0266(13) Uani 1 1 d .
N4 N 0.7396(6) 1.2358(4) 1.2220(4) 0.0282(13) Uani 1 1 d .
O1 O 0.4685(6) 1.3044(5) 0.5911(4) 0.0509(15) Uani 1 1 d .
O2 O 0.2058(5) 1.3861(4) 1.3466(4) 0.0390(12) Uani 1 1 d .
O3 O 1.2198(5) 1.3890(4) 0.9448(4) 0.0367(12) Uani 1 1 d .
O4 O 0.8531(6) 1.3065(6) 1.6383(4) 0.0612(17) Uani 1 1 d .
O01 O 0.4249(5) 0.9993(3) 0.8575(3) 0.0256(10) Uiso 1 1 d .
O02 O 0.6711(5) 1.0011(3) 0.9708(3) 0.0251(10) Uiso 1 1 d .
C1 C 0.2810(16) 0.9982(11) 0.8429(11) 0.102(4) Uiso 1 1 d .
C2 C 0.1869(16) 0.9969(10) 0.7566(11) 0.102(4) Uiso 1 1 d .
H2A H 0.2152 0.9961 0.7019 0.123 Uiso 1 1 calc R
C3 C 0.0669(15) 0.9966(10) 0.7433(11) 0.093(4) Uiso 1 1 d .
H3A H 0.0069 0.9945 0.6794 0.112 Uiso 1 1 calc R
C4 C 0.0147(17) 0.9996(11) 0.8253(12) 0.108(4) Uiso 1 1 d .
H4A H -0.0767 1.0012 0.8152 0.129 Uiso 1 1 calc R
C5 C 0.7646(15) 1.0005(10) 1.0698(11) 0.096(4) Uiso 1 1 d .
C6 C 0.9016(16) 0.9999(11) 1.0875(12) 0.105(4) Uiso 1 1 d .
H6A H 0.9346 0.9991 1.0350 0.126 Uiso 1 1 calc R
C10 C 0.4508(7) 1.2672(5) 1.0116(5) 0.0283(16) Uani 1 1 d .
H10A H 0.4075 1.3132 0.9986 0.034 Uiso 1 1 calc R
C11 C 0.4993(4) 1.2550(4) 0.8622(3) 0.0264(15) Uani 1 1 d G
C12 C 0.3737(4) 1.2621(4) 0.8032(3) 0.0387(18) Uani 1 1 d G
H12A H 0.2980 1.2554 0.8248 0.046 Uiso 1 1 calc R
C13 C 0.3599(4) 1.2791(4) 0.7123(3) 0.044(2) Uani 1 1 d G
H13A H 0.2749 1.2839 0.6724 0.052 Uiso 1 1 calc R
C14 C 0.4718(5) 1.2890(4) 0.6803(3) 0.0367(18) Uani 1 1 d G
C15 C 0.5975(4) 1.2819(4) 0.7393(3) 0.0371(18) Uani 1 1 d G
H15A H 0.6732 1.2886 0.7176 0.045 Uiso 1 1 calc R
C16 C 0.6112(4) 1.2650(4) 0.8302(3) 0.0312(16) Uani 1 1 d G
H16A H 0.6962 1.2602 0.8701 0.037 Uiso 1 1 calc R
C17 C 0.3385(11) 1.3031(10) 0.5237(7) 0.080(3) Uani 1 1 d .
H17A H 0.3502 1.3146 0.4640 0.119 Uiso 1 1 calc R
H17B H 0.3156 1.3573 0.5600 0.119 Uiso 1 1 calc R
H17C H 0.2604 1.2367 0.5007 0.119 Uiso 1 1 calc R
C21 C 0.3899(4) 1.2778(3) 1.1546(3) 0.0250(15) Uani 1 1 d G
C22 C 0.2846(5) 1.2110(2) 1.1712(3) 0.0340(17) Uani 1 1 d G
H22A H 0.2530 1.1392 1.1382 0.041 Uiso 1 1 calc R
C23 C 0.2260(4) 1.2503(3) 1.2368(3) 0.0357(17) Uani 1 1 d G
H23A H 0.1548 1.2051 1.2480 0.043 Uiso 1 1 calc R
C24 C 0.2727(5) 1.3563(3) 1.2857(3) 0.0307(16) Uani 1 1 d G
C25 C 0.3780(5) 1.4232(2) 1.2690(3) 0.0355(17) Uani 1 1 d G
H25A H 0.4096 1.4949 1.3021 0.043 Uiso 1 1 calc R
C26 C 0.4366(4) 1.3839(3) 1.2035(3) 0.0335(17) Uani 1 1 d G
H26A H 0.5079 1.4291 1.1922 0.040 Uiso 1 1 calc R
C27 C 0.2530(11) 1.4921(7) 1.4012(8) 0.062(3) Uani 1 1 d .
H27A H 0.1979 1.5033 1.4416 0.093 Uiso 1 1 calc R
H27B H 0.2389 1.5264 1.3525 0.093 Uiso 1 1 calc R
H27C H 0.3550 1.5201 1.4472 0.093 Uiso 1 1 calc R
C30 C 0.8418(7) 1.2719(5) 1.1912(5) 0.0285(16) Uani 1 1 d .
H30A H 0.9350 1.3200 1.2397 0.034 Uiso 1 1 calc R
C31 C 0.9168(4) 1.2815(3) 1.0563(3) 0.0229(14) Uani 1 1 d G
C32 C 0.9402(4) 1.2147(2) 0.9831(3) 0.0326(16) Uani 1 1 d G
H32A H 0.8867 1.1431 0.9577 0.039 Uiso 1 1 calc R
C33 C 1.0425(5) 1.2536(3) 0.9474(3) 0.0364(17) Uani 1 1 d G
H33A H 1.0582 1.2084 0.8979 0.044 Uiso 1 1 calc R
C34 C 1.1215(4) 1.3594(3) 0.9849(3) 0.0292(16) Uani 1 1 d G
C35 C 1.0982(4) 1.4263(2) 1.0581(3) 0.0336(17) Uani 1 1 d G
H35A H 1.1516 1.4978 1.0835 0.040 Uiso 1 1 calc R
C36 C 0.9958(5) 1.3873(3) 1.0938(3) 0.0317(16) Uani 1 1 d G
H36A H 0.9801 1.4325 1.1433 0.038 Uiso 1 1 calc R
C37 C 1.3043(9) 1.4955(6) 0.9813(7) 0.050(2) Uani 1 1 d .
H37A H 1.3696 1.5065 0.9477 0.075 Uiso 1 1 calc R
H37B H 1.3600 1.5216 1.0558 0.075 Uiso 1 1 calc R
H37C H 1.2413 1.5316 0.9658 0.075 Uiso 1 1 calc R
C41 C 0.7778(4) 1.2589(4) 1.3308(2) 0.0290(16) Uani 1 1 d G
C42 C 0.9153(4) 1.2769(5) 1.3994(3) 0.048(2) Uani 1 1 d G
H42A H 0.9887 1.2784 1.3760 0.057 Uiso 1 1 calc R
C43 C 0.9444(4) 1.2927(5) 1.5027(3) 0.055(2) Uani 1 1 d G
H43A H 1.0375 1.3049 1.5491 0.066 Uiso 1 1 calc R
C44 C 0.8360(5) 1.2905(5) 1.5374(2) 0.0409(19) Uani 1 1 d G
C45 C 0.6984(4) 1.2725(4) 1.4687(3) 0.0417(19) Uani 1 1 d G
H45A H 0.6251 1.2710 1.4921 0.050 Uiso 1 1 calc R
C46 C 0.6693(4) 1.2567(4) 1.3654(3) 0.0362(18) Uani 1 1 d G
H46A H 0.5763 1.2444 1.3190 0.043 Uiso 1 1 calc R
C47 C 0.9906(12) 1.3276(12) 1.7121(7) 0.095(4) Uani 1 1 d .
H47A H 0.9873 1.3359 1.7789 0.142 Uiso 1 1 calc R
H47B H 1.0606 1.3906 1.7175 0.142 Uiso 1 1 calc R
H47C H 1.0189 1.2708 1.6907 0.142 Uiso 1 1 calc R
Cl1 Cl 0.3713(11) 0.9950(8) 0.2835(8) 0.146(3) Uiso 0.50 1 d PD
Cl2 Cl 0.311(3) 1.010(2) 0.461(2) 0.363(13) Uiso 0.50 1 d PD
C1S C 0.273(6) 0.925(3) 0.336(3) 0.28(3) Uiso 0.50 1 d PD
H1SA H 0.3010 0.8675 0.3419 0.333 Uiso 0.50 1 calc PR
H1SB H 0.1688 0.8965 0.2917 0.333 Uiso 0.50 1 calc PR
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
N3 Mo1 N1 94.8(2) . .
N3 Mo1 Mo2 91.79(15) . .
N1 Mo1 Mo2 92.96(14) . .
N3 Mo1 O01 163.76(19) . .
N1 Mo1 O01 92.81(19) . .
Mo2 Mo1 O01 102.13(12) . .
N3 Mo1 O02 94.09(19) . .
N1 Mo1 O02 162.86(19) . .
Mo2 Mo1 O02 101.37(12) . .
O01 Mo1 O02 75.14(16) . .
N2 Mo2 N4 94.7(2) . .
N2 Mo2 Mo1 91.56(15) . .
N4 Mo2 Mo1 92.67(15) . .
N2 Mo2 O01 163.47(19) . 2_677
N4 Mo2 O01 93.20(19) . 2_677
Mo1 Mo2 O01 102.57(12) . 2_677
N2 Mo2 O02 93.69(19) . 2_677
N4 Mo2 O02 163.05(19) . 2_677
Mo1 Mo2 O02 101.81(12) . 2_677
O01 Mo2 O02 75.22(17) 2_677 2_677
C10 N1 C11 119.0(5) . .
C10 N1 Mo1 117.4(4) . .
C11 N1 Mo1 122.5(4) . .
C10 N2 C21 118.8(5) . .
C10 N2 Mo2 119.2(4) . .
C21 N2 Mo2 122.0(4) . .
C30 N3 C31 118.8(5) . .
C30 N3 Mo1 119.0(4) . .
C31 N3 Mo1 122.2(4) . .
C30 N4 C41 119.2(5) . .
C30 N4 Mo2 118.1(4) . .
C41 N4 Mo2 121.8(4) . .
C14 O1 C17 117.7(6) . .
C24 O2 C27 117.3(6) . .
C34 O3 C37 117.3(5) . .
C44 O4 C47 117.9(6) . .
C1 O01 Mo2 115.2(6) . 2_677
C1 O01 Mo1 115.4(6) . .
Mo2 O01 Mo1 100.13(18) 2_677 .
C5 O02 Mo2 113.7(6) . 2_677
C5 O02 Mo1 115.0(6) . .
Mo2 O02 Mo1 99.42(18) 2_677 .
C2 C1 O01 124.2(13) . .
C2 C1 C5 117.2(13) . 2_677
O01 C1 C5 118.6(11) . 2_677
C3 C2 C1 125.1(16) . .
C2 C3 C4 121.2(14) . .
C6 C4 C3 118.4(14) 2_677 .
C6 C5 O02 121.6(12) . .
C6 C5 C1 116.0(13) . 2_677
O02 C5 C1 122.4(11) . 2_677
C4 C6 C5 122.1(15) 2_677 .
N2 C10 N1 118.8(6) . .
C12 C11 C16 120.0 . .
C12 C11 N1 121.7(3) . .
C16 C11 N1 118.2(3) . .
C11 C12 C13 120.0 . .
C14 C13 C12 120.0 . .
O1 C14 C13 124.7(4) . .
O1 C14 C15 115.3(4) . .
C13 C14 C15 120.0 . .
C14 C15 C16 120.0 . .
C15 C16 C11 120.0 . .
C22 C21 C26 120.0 . .
C22 C21 N2 118.6(3) . .
C26 C21 N2 121.4(3) . .
C23 C22 C21 120.0 . .
C24 C23 C22 120.0 . .
O2 C24 C25 125.1(4) . .
O2 C24 C23 114.9(3) . .
C25 C24 C23 120.0 . .
C24 C25 C26 120.0 . .
C25 C26 C21 120.0 . .
N3 C30 N4 118.4(6) . .
C32 C31 C36 120.0 . .
C32 C31 N3 118.5(3) . .
C36 C31 N3 121.5(3) . .
C31 C32 C33 120.0 . .
C32 C33 C34 120.0 . .
O3 C34 C35 125.0(3) . .
O3 C34 C33 115.0(3) . .
C35 C34 C33 120.0 . .
C34 C35 C36 120.0 . .
C35 C36 C31 120.0 . .
C42 C41 C46 120.0 . .
C42 C41 N4 122.2(3) . .
C46 C41 N4 117.7(3) . .
C43 C42 C41 120.0 . .
C42 C43 C44 120.0 . .
O4 C44 C43 124.9(4) . .
O4 C44 C45 115.1(4) . .
C43 C44 C45 120.0 . .
C46 C45 C44 120.0 . .
C45 C46 C41 120.0 . .
Cl1 C1S Cl2 108(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 N3 2.103(6) .
Mo1 N1 2.104(6) .
Mo1 Mo2 2.1135(9) .
Mo1 O01 2.131(4) .
Mo1 O02 2.142(4) .
Mo2 N2 2.098(5) .
Mo2 N4 2.104(6) .
Mo2 O01 2.129(4) 2_677
Mo2 O02 2.140(4) 2_677
N1 C10 1.330(9) .
N1 C11 1.431(6) .
N2 C10 1.319(9) .
N2 C21 1.425(6) .
N3 C30 1.324(8) .
N3 C31 1.434(6) .
N4 C30 1.327(9) .
N4 C41 1.438(6) .
O1 C14 1.375(5) .
O1 C17 1.413(11) .
O2 C24 1.365(5) .
O2 C27 1.401(10) .
O3 C34 1.370(5) .
O3 C37 1.410(9) .
O4 C44 1.383(6) .
O4 C47 1.405(11) .
O01 C1 1.465(15) .
O01 Mo2 2.129(4) 2_677
O02 C5 1.483(15) .
O02 Mo2 2.140(4) 2_677
C1 C2 1.335(18) .
C1 C5 1.503(19) 2_677
C2 C3 1.223(17) .
C3 C4 1.470(19) .
C4 C6 1.307(18) 2_677
C5 C6 1.394(19) .
C5 C1 1.503(19) 2_677
C6 C4 1.307(18) 2_677
C11 C12 1.3900 .
C11 C16 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C14 C15 1.3900 .
C15 C16 1.3900 .
C21 C22 1.3900 .
C21 C26 1.3900 .
C22 C23 1.3900 .
C23 C24 1.3900 .
C24 C25 1.3900 .
C25 C26 1.3900 .
C31 C32 1.3900 .
C31 C36 1.3900 .
C32 C33 1.3900 .
C33 C34 1.3900 .
C34 C35 1.3900 .
C35 C36 1.3900 .
C41 C42 1.3900 .
C41 C46 1.3900 .
C42 C43 1.3900 .
C43 C44 1.3900 .
C44 C45 1.3900 .
C45 C46 1.3900 .
Cl1 C1S 1.75(2) .
Cl2 C1S 1.77(2) .
