#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/88/1518803.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_1518803
loop_
_publ_author_name
'Irene Mendoza'
'Natalia Curado'
'Mario Carrasco'
'Eleuterio Alvarez'
'Riccardo Peloso'
'Amor Rodriguez'
'Ernesto Carmona'
_publ_section_title
;
 Synthesis and structure of mixed carboxylate-aminopyridinate and
 -amidinate complexes of dimolybdenum and ditungsten
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120
_journal_page_last               128
_journal_volume                  424
_journal_year                    2015
_chemical_formula_moiety         'C46 H48 Mo2 N4 O4'
_chemical_formula_sum            'C46 H48 Mo2 N4 O4'
_chemical_formula_weight         912.76
_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
_cell_angle_alpha                109.5150(10)
_cell_angle_beta                 94.1570(10)
_cell_angle_gamma                107.9920(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6189(2)
_cell_length_b                   10.2292(2)
_cell_length_c                   12.1372(3)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.69
_cell_measurement_theta_min      2.57
_cell_volume                     1049.82(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.798
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_correction_T_min  0.8819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0360P)²+0.4234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                7492
_reflns_number_total             8115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2015-424-120-128-5.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_database_code               1518803
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 1.017650(10) 0.557359(10) 0.591873(8) 0.01122(3) Uani 1 1 d .
O1 O 1.18969(9) 0.47883(10) 0.62402(8) 0.01511(15) Uani 1 1 d .
O2 O 0.84230(10) 0.63709(10) 0.57228(8) 0.01620(15) Uani 1 1 d .
N1 N 0.86557(11) 0.36705(11) 0.61340(8) 0.01335(16) Uani 1 1 d .
N2 N 0.82755(11) 0.24326(11) 0.41068(8) 0.01333(16) Uani 1 1 d .
C22 C 0.77872(13) 0.60527(14) 0.46618(11) 0.0165(2) Uani 1 1 d .
C23 C 0.66302(16) 0.66978(18) 0.44694(13) 0.0284(3) Uani 1 1 d .
H23A H 0.6582 0.6763 0.3681 0.043 Uiso 1 1 calc R
H23B H 0.6895 0.7691 0.5084 0.043 Uiso 1 1 calc R
H23C H 0.5657 0.6060 0.4517 0.043 Uiso 1 1 calc R
C1 C 0.79632(13) 0.23791(13) 0.51573(10) 0.01421(19) Uani 1 1 d .
C2 C 0.69970(15) 0.11175(14) 0.53192(11) 0.0210(2) Uani 1 1 d .
H2 H 0.6513 0.0216 0.4654 0.025 Uiso 1 1 calc R
C3 C 0.67683(17) 0.12090(16) 0.64382(12) 0.0277(3) Uani 1 1 d .
H3 H 0.6124 0.0367 0.6548 0.033 Uiso 1 1 calc R
C4 C 0.74847(16) 0.25487(16) 0.74327(12) 0.0253(3) Uani 1 1 d .
H4 H 0.7325 0.2623 0.8211 0.030 Uiso 1 1 calc R
C5 C 0.84131(13) 0.37330(14) 0.72422(10) 0.0159(2) Uani 1 1 d .
C6 C 0.92649(13) 0.52275(13) 0.81861(10) 0.01456(19) Uani 1 1 d .
C7 C 1.07359(13) 0.55419(13) 0.87209(10) 0.01492(19) Uani 1 1 d .
C12 C 1.13552(15) 0.43260(15) 0.85836(11) 0.0204(2) Uani 1 1 d .
H12A H 1.2445 0.4756 0.8806 0.031 Uiso 1 1 calc R
H12B H 1.1059 0.3627 0.7753 0.031 Uiso 1 1 calc R
H12C H 1.0964 0.3802 0.9103 0.031 Uiso 1 1 calc R
C8 C 1.16074(14) 0.70070(14) 0.94216(11) 0.0195(2) Uani 1 1 d .
H8 H 1.2615 0.7239 0.9765 0.023 Uiso 1 1 calc R
C9 C 1.10281(17) 0.81315(15) 0.96262(12) 0.0258(3) Uani 1 1 d .
H9 H 1.1644 0.9130 1.0083 0.031 Uiso 1 1 calc R
C10 C 0.95433(17) 0.77897(16) 0.91593(13) 0.0252(3) Uani 1 1 d .
H10 H 0.9135 0.8555 0.9334 0.030 Uiso 1 1 calc R
C11 C 0.86418(14) 0.63428(15) 0.84389(11) 0.0194(2) Uani 1 1 d .
C13 C 0.70256(16) 0.5985(2) 0.79484(14) 0.0307(3) Uani 1 1 d .
H13A H 0.6766 0.6875 0.8272 0.046 Uiso 1 1 calc R
H13B H 0.6398 0.5201 0.8178 0.046 Uiso 1 1 calc R
H13C H 0.6862 0.5648 0.7077 0.046 Uiso 1 1 calc R
C14 C 0.75284(12) 0.11380(12) 0.30518(10) 0.01358(18) Uani 1 1 d .
C19 C 0.81610(14) 0.00386(14) 0.26409(12) 0.0194(2) Uani 1 1 d .
C21 C 0.95902(17) 0.01486(17) 0.33272(16) 0.0323(3) Uani 1 1 d .
H21A H 0.9769 -0.0784 0.2982 0.048 Uiso 1 1 calc R
H21B H 0.9510 0.0337 0.4162 0.048 Uiso 1 1 calc R
H21C H 1.0420 0.0964 0.3284 0.048 Uiso 1 1 calc R
C18 C 0.74357(16) -0.11764(15) 0.15815(13) 0.0246(3) Uani 1 1 d .
H18 H 0.7858 -0.1922 0.1294 0.030 Uiso 1 1 calc R
C17 C 0.61104(16) -0.13127(15) 0.09422(12) 0.0240(3) Uani 1 1 d .
H17 H 0.5635 -0.2141 0.0219 0.029 Uiso 1 1 calc R
C16 C 0.54845(14) -0.02382(15) 0.13616(11) 0.0198(2) Uani 1 1 d .
H16 H 0.4570 -0.0341 0.0927 0.024 Uiso 1 1 calc R
C15 C 0.61756(12) 0.09955(13) 0.24141(10) 0.01495(19) Uani 1 1 d .
C20 C 0.54545(14) 0.21347(15) 0.28468(13) 0.0228(2) Uani 1 1 d .
H20A H 0.5928 0.2978 0.2621 0.034 Uiso 1 1 calc R
H20B H 0.5574 0.2476 0.3716 0.034 Uiso 1 1 calc R
H20C H 0.4391 0.1693 0.2485 0.034 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'
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'
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
Mo1 Mo1 O1 91.84(2) 2_766 .
Mo1 Mo1 O2 91.86(2) 2_766 .
O1 Mo1 O2 175.80(3) . .
Mo1 Mo1 N2 94.24(3) 2_766 2_766
O1 Mo1 N2 92.18(4) . 2_766
O2 Mo1 N2 89.50(4) . 2_766
Mo1 Mo1 N1 91.45(3) 2_766 .
O1 Mo1 N1 87.35(4) . .
O2 Mo1 N1 90.60(4) . .
N2 Mo1 N1 174.31(3) 2_766 .
C22 O1 Mo1 117.10(7) 2_766 .
C22 O2 Mo1 116.75(8) . .
C5 N1 C1 120.11(10) . .
C5 N1 Mo1 120.07(8) . .
C1 N1 Mo1 119.79(7) . .
C1 N2 C14 117.81(9) . .
C1 N2 Mo1 119.00(7) . 2_766
C14 N2 Mo1 123.19(7) . 2_766
O1 C22 O2 122.26(11) 2_766 .
O1 C22 C23 118.80(11) 2_766 .
O2 C22 C23 118.94(11) . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N2 C1 N1 115.49(10) . .
N2 C1 C2 125.39(11) . .
N1 C1 C2 119.12(10) . .
C3 C2 C1 119.68(12) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C2 C3 C4 120.46(12) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C5 C4 C3 118.13(12) . .
C5 C4 H4 120.9 . .
C3 C4 H4 120.9 . .
N1 C5 C4 122.50(11) . .
N1 C5 C6 112.12(10) . .
C4 C5 C6 125.38(11) . .
C11 C6 C7 120.63(11) . .
C11 C6 C5 119.58(11) . .
C7 C6 C5 119.47(11) . .
C8 C7 C6 118.67(11) . .
C8 C7 C12 120.06(11) . .
C6 C7 C12 121.23(11) . .
C7 C12 H12A 109.5 . .
C7 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C7 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C9 C8 C7 121.06(12) . .
C9 C8 H8 119.5 . .
C7 C8 H8 119.5 . .
C8 C9 C10 119.60(13) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C9 C10 C11 121.04(12) . .
C9 C10 H10 119.5 . .
C11 C10 H10 119.5 . .
C10 C11 C6 118.72(12) . .
C10 C11 C13 120.44(13) . .
C6 C11 C13 120.84(13) . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 C19 120.23(11) . .
C15 C14 N2 119.39(10) . .
C19 C14 N2 120.36(10) . .
C18 C19 C14 118.84(11) . .
C18 C19 C21 120.02(12) . .
C14 C19 C21 121.14(11) . .
C19 C21 H21A 109.5 . .
C19 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C19 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C17 C18 C19 121.13(12) . .
C17 C18 H18 119.4 . .
C19 C18 H18 119.4 . .
C16 C17 C18 119.67(12) . .
C16 C17 H17 120.2 . .
C18 C17 H17 120.2 . .
C17 C16 C15 121.02(11) . .
C17 C16 H16 119.5 . .
C15 C16 H16 119.5 . .
C16 C15 C14 119.11(11) . .
C16 C15 C20 119.47(11) . .
C14 C15 C20 121.42(11) . .
C15 C20 H20A 109.5 . .
C15 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C15 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 Mo1 2.08844(18) 2_766
Mo1 O1 2.1149(9) .
Mo1 O2 2.1184(9) .
Mo1 N2 2.1332(10) 2_766
Mo1 N1 2.1526(10) .
O1 C22 1.2694(15) 2_766
O2 C22 1.2731(14) .
N1 C5 1.3656(15) .
N1 C1 1.3747(15) .
N2 C1 1.3457(14) .
N2 C14 1.4337(14) .
N2 Mo1 2.1332(10) 2_766
C22 O1 1.2694(15) 2_766
C22 C23 1.4991(18) .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C1 C2 1.4222(17) .
C2 C3 1.3686(18) .
C2 H2 0.9500 .
C3 C4 1.4145(19) .
C3 H3 0.9500 .
C4 C5 1.3665(18) .
C4 H4 0.9500 .
C5 C6 1.4970(17) .
C6 C11 1.4036(17) .
C6 C7 1.4046(16) .
C7 C8 1.3932(17) .
C7 C12 1.5044(17) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C8 C9 1.3858(19) .
C8 H8 0.9500 .
C9 C10 1.387(2) .
C9 H9 0.9500 .
C10 C11 1.393(2) .
C10 H10 0.9500 .
C11 C13 1.5080(18) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.4054(15) .
C14 C19 1.4055(17) .
C19 C18 1.3969(18) .
C19 C21 1.5074(18) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C18 C17 1.386(2) .
C18 H18 0.9500 .
C17 C16 1.382(2) .
C17 H17 0.9500 .
C16 C15 1.3957(16) .
C16 H16 0.9500 .
C15 C20 1.5026(17) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 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
Mo1 Mo1 O1 C22 0.47(8) 2_766 2_766
O2 Mo1 O1 C22 152.5(4) . 2_766
N2 Mo1 O1 C22 -93.84(9) 2_766 2_766
N1 Mo1 O1 C22 91.84(9) . 2_766
Mo1 Mo1 O2 C22 -4.25(9) 2_766 .
O1 Mo1 O2 C22 -156.3(4) . .
N2 Mo1 O2 C22 89.97(9) 2_766 .
N1 Mo1 O2 C22 -95.72(9) . .
Mo1 Mo1 N1 C5 178.85(9) 2_766 .
O1 Mo1 N1 C5 87.07(9) . .
O2 Mo1 N1 C5 -89.27(9) . .
N2 Mo1 N1 C5 1.7(4) 2_766 .
Mo1 Mo1 N1 C1 0.74(9) 2_766 .
O1 Mo1 N1 C1 -91.04(9) . .
O2 Mo1 N1 C1 92.62(9) . .
N2 Mo1 N1 C1 -176.4(3) 2_766 .
Mo1 O2 C22 O1 4.94(16) . 2_766
Mo1 O2 C22 C23 -174.78(10) . .
C14 N2 C1 N1 -177.09(9) . .
Mo1 N2 C1 N1 2.17(14) 2_766 .
C14 N2 C1 C2 2.94(18) . .
Mo1 N2 C1 C2 -177.80(10) 2_766 .
C5 N1 C1 N2 179.99(10) . .
Mo1 N1 C1 N2 -1.90(14) . .
C5 N1 C1 C2 -0.04(17) . .
Mo1 N1 C1 C2 178.07(9) . .
N2 C1 C2 C3 -179.80(13) . .
N1 C1 C2 C3 0.2(2) . .
C1 C2 C3 C4 0.1(2) . .
C2 C3 C4 C5 -0.5(2) . .
C1 N1 C5 C4 -0.47(19) . .
Mo1 N1 C5 C4 -178.57(11) . .
C1 N1 C5 C6 179.93(10) . .
Mo1 N1 C5 C6 1.83(14) . .
C3 C4 C5 N1 0.7(2) . .
C3 C4 C5 C6 -179.71(13) . .
N1 C5 C6 C11 86.58(14) . .
C4 C5 C6 C11 -93.01(16) . .
N1 C5 C6 C7 -86.96(13) . .
C4 C5 C6 C7 93.45(16) . .
C11 C6 C7 C8 -5.71(17) . .
C5 C6 C7 C8 167.75(11) . .
C11 C6 C7 C12 172.13(11) . .
C5 C6 C7 C12 -14.41(16) . .
C6 C7 C8 C9 2.25(19) . .
C12 C7 C8 C9 -175.62(12) . .
C7 C8 C9 C10 2.1(2) . .
C8 C9 C10 C11 -3.1(2) . .
C9 C10 C11 C6 -0.3(2) . .
C9 C10 C11 C13 179.35(13) . .
C7 C6 C11 C10 4.74(18) . .
C5 C6 C11 C10 -168.72(11) . .
C7 C6 C11 C13 -174.88(11) . .
C5 C6 C11 C13 11.66(17) . .
C1 N2 C14 C15 91.53(13) . .
Mo1 N2 C14 C15 -87.70(12) 2_766 .
C1 N2 C14 C19 -90.10(14) . .
Mo1 N2 C14 C19 90.67(12) 2_766 .
C15 C14 C19 C18 1.14(19) . .
N2 C14 C19 C18 -177.21(12) . .
C15 C14 C19 C21 -178.39(12) . .
N2 C14 C19 C21 3.25(19) . .
C14 C19 C18 C17 -0.4(2) . .
C21 C19 C18 C17 179.17(14) . .
C19 C18 C17 C16 -0.6(2) . .
C18 C17 C16 C15 0.8(2) . .
C17 C16 C15 C14 -0.03(18) . .
C17 C16 C15 C20 -179.53(12) . .
C19 C14 C15 C16 -0.95(17) . .
N2 C14 C15 C16 177.42(10) . .
C19 C14 C15 C20 178.54(12) . .
N2 C14 C15 C20 -3.09(17) . .
