#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:38:45 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180149 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/46/7104626.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_7104626
loop_
_publ_author_name
'Nippe, Michael'
'Timmer, George H'
'Berry, John F'
_publ_section_title
;
 Remarkable regioselectivity in the preparation of the first
 heterotrimetallic Mo[quadruple bond]W...Cr chain.
;
_journal_issue                   29
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4357
_journal_page_last               4359
_journal_paper_doi               10.1039/b907402c
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C40 H32 Mo N12 W '
_chemical_formula_sum            'C40 H32 Mo N12 W'
_chemical_formula_weight         960.57
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 101.246(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1454(6)
_cell_length_b                   11.5144(4)
_cell_length_c                   16.6938(5)
_cell_measurement_reflns_used    7840
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.1073
_cell_measurement_theta_min      4.5738
_cell_volume                     3420.92(19)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50° ω and 0.5 ° φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6195
_diffrn_reflns_theta_full        69.88
_diffrn_reflns_theta_max         69.88
_diffrn_reflns_theta_min         4.57
_exptl_absorpt_coefficient_mu    9.540
_exptl_absorpt_correction_T_max  0.8470
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         6195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0401
_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)+(0.0526P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                4871
_reflns_number_total             6195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907402c.txt
_cod_data_source_block           MoW
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7104626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.5000 0.93288(3) 0.7500 0.01203(8) Uani 0.5195(12) 2 d SP . 1
W1A W 0.5000 0.74745(3) 0.7500 0.01203(8) Uani 0.4805(12) 2 d SP . 2
Mo1 Mo 0.5000 0.74745(3) 0.7500 0.01203(8) Uani 0.5195(12) 2 d SP . 1
Mo1A Mo 0.5000 0.93288(3) 0.7500 0.01203(8) Uani 0.4805(12) 2 d SP . 2
N1 N 0.4551(2) 0.7377(3) 0.8603(2) 0.0137(8) Uani 1 1 d . . .
N2 N 0.44901(19) 0.9371(3) 0.8562(2) 0.0148(8) Uani 1 1 d . . .
N3 N 0.4492(2) 1.1252(3) 0.8227(2) 0.0183(8) Uani 1 1 d . . .
N4 N 0.6008(2) 0.5433(3) 0.8313(2) 0.0182(8) Uani 1 1 d . . .
N5 N 0.6131(2) 0.7400(3) 0.8168(2) 0.0140(8) Uani 1 1 d . . .
N6 N 0.6109(2) 0.9397(3) 0.8250(2) 0.0153(8) Uani 1 1 d . . .
C10 C 0.4472(2) 0.6352(4) 0.8975(3) 0.0162(10) Uani 1 1 d . . .
H10A H 0.4676 0.5674 0.8776 0.019 Uiso 1 1 calc R . .
C11 C 0.4116(2) 0.6238(4) 0.9621(3) 0.0178(10) Uani 1 1 d . . .
H11A H 0.4105 0.5514 0.9892 0.021 Uiso 1 1 calc R . .
C12 C 0.3770(2) 0.7220(4) 0.9868(3) 0.0189(10) Uani 1 1 d . . .
H12A H 0.3476 0.7156 1.0279 0.023 Uiso 1 1 calc R . .
C13 C 0.3854(2) 0.8273(4) 0.9521(3) 0.0181(9) Uani 1 1 d . . .
H13A H 0.3614 0.8940 0.9688 0.022 Uiso 1 1 calc R . .
C14 C 0.4296(2) 0.8376(4) 0.8915(3) 0.0153(9) Uani 1 1 d . . .
C30 C 0.4383(2) 1.0497(4) 0.8810(3) 0.0147(10) Uani 1 1 d . . .
C31 C 0.4238(2) 1.0905(4) 0.9562(3) 0.0164(10) Uani 1 1 d . . .
H31A H 0.4192 1.0375 0.9985 0.020 Uiso 1 1 calc R . .
C32 C 0.4164(3) 1.2084(4) 0.9672(3) 0.0196(10) Uani 1 1 d . . .
H32A H 0.4058 1.2372 1.0171 0.024 Uiso 1 1 calc R . .
C33 C 0.4243(3) 1.2844(4) 0.9053(3) 0.0209(10) Uani 1 1 d . . .
H33A H 0.4174 1.3656 0.9107 0.025 Uiso 1 1 calc R . .
C34 C 0.4423(3) 1.2384(4) 0.8359(3) 0.0209(10) Uani 1 1 d . . .
H34A H 0.4505 1.2908 0.7945 0.025 Uiso 1 1 calc R . .
C40 C 0.6475(2) 0.6309(4) 0.8206(2) 0.0148(9) Uani 1 1 d . . .
C41 C 0.7202(2) 0.6106(4) 0.8076(3) 0.0184(9) Uani 1 1 d . . .
H41A H 0.7518 0.6738 0.8000 0.022 Uiso 1 1 calc R . .
C42 C 0.7455(2) 0.4987(4) 0.8059(3) 0.0224(10) Uani 1 1 d . . .
H42A H 0.7944 0.4836 0.7961 0.027 Uiso 1 1 calc R . .
C43 C 0.6990(3) 0.4078(4) 0.8185(3) 0.0219(11) Uani 1 1 d . . .
H43A H 0.7155 0.3294 0.8189 0.026 Uiso 1 1 calc R . .
C44 C 0.6284(3) 0.4352(4) 0.8305(3) 0.0209(10) Uani 1 1 d . . .
H44A H 0.5965 0.3728 0.8389 0.025 Uiso 1 1 calc R . .
C60 C 0.6441(2) 1.0419(4) 0.8546(3) 0.0164(10) Uani 1 1 d . . .
H60A H 0.6180 1.1123 0.8385 0.020 Uiso 1 1 calc R . .
C61 C 0.7121(2) 1.0482(4) 0.9057(3) 0.0198(10) Uani 1 1 d . . .
H61A H 0.7333 1.1213 0.9238 0.024 Uiso 1 1 calc R . .
C62 C 0.7504(3) 0.9451(4) 0.9312(3) 0.0227(10) Uani 1 1 d . . .
H62A H 0.7971 0.9474 0.9686 0.027 Uiso 1 1 calc R . .
C63 C 0.7201(2) 0.8412(4) 0.9021(3) 0.0194(9) Uani 1 1 d . . .
H63A H 0.7461 0.7710 0.9190 0.023 Uiso 1 1 calc R . .
C64 C 0.6500(2) 0.8379(4) 0.8467(2) 0.0138(9) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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
N2 W1 N2 177.43(19) 2_656 . ?
N2 W1 N6 88.56(13) 2_656 . ?
N2 W1 N6 91.34(13) . . ?
N2 W1 N6 91.34(13) 2_656 2_656 ?
N2 W1 N6 88.56(13) . 2_656 ?
N6 W1 N6 175.8(2) . 2_656 ?
N5 W1A N5 175.39(19) 2_656 . ?
N5 W1A N1 87.70(14) 2_656 . ?
N5 W1A N1 92.06(14) . . ?
N5 W1A N1 92.06(14) 2_656 2_656 ?
N5 W1A N1 87.70(14) . 2_656 ?
N1 W1A N1 174.03(18) . 2_656 ?
C10 N1 C14 118.7(4) . . ?
C10 N1 W1A 121.9(3) . . ?
C14 N1 W1A 119.3(3) . . ?
C14 N2 C30 126.4(4) . . ?
C14 N2 W1 121.6(3) . . ?
C30 N2 W1 112.0(3) . . ?
C34 N3 C30 118.6(4) . . ?
C44 N4 C40 116.5(4) . . ?
C64 N5 C40 123.1(4) . . ?
C64 N5 W1A 120.9(3) . . ?
C40 N5 W1A 115.7(3) . . ?
C60 N6 C64 117.9(4) . . ?
C60 N6 W1 122.4(3) . . ?
C64 N6 W1 119.7(3) . . ?
N1 C10 C11 123.6(4) . . ?
N1 C10 H10A 118.2 . . ?
C11 C10 H10A 118.2 . . ?
C10 C11 C12 117.7(4) . . ?
C10 C11 H11A 121.1 . . ?
C12 C11 H11A 121.1 . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
N2 C14 N1 113.8(4) . . ?
N2 C14 C13 127.5(4) . . ?
N1 C14 C13 118.6(4) . . ?
N3 C30 N2 109.8(4) . . ?
N3 C30 C31 120.5(4) . . ?
N2 C30 C31 129.6(4) . . ?
C32 C31 C30 119.0(4) . . ?
C32 C31 H31A 120.5 . . ?
C30 C31 H31A 120.5 . . ?
C31 C32 C33 119.7(4) . . ?
C31 C32 H32A 120.1 . . ?
C33 C32 H32A 120.1 . . ?
C34 C33 C32 117.7(4) . . ?
C34 C33 H33A 121.2 . . ?
C32 C33 H33A 121.2 . . ?
N3 C34 C33 124.3(4) . . ?
N3 C34 H34A 117.8 . . ?
C33 C34 H34A 117.8 . . ?
N4 C40 N5 113.0(4) . . ?
N4 C40 C41 122.0(4) . . ?
N5 C40 C41 124.7(4) . . ?
C42 C41 C40 119.4(4) . . ?
C42 C41 H41A 120.3 . . ?
C40 C41 H41A 120.3 . . ?
C41 C42 C43 119.4(4) . . ?
C41 C42 H42A 120.3 . . ?
C43 C42 H42A 120.3 . . ?
C44 C43 C42 117.5(4) . . ?
C44 C43 H43A 121.2 . . ?
C42 C43 H43A 121.2 . . ?
N4 C44 C43 125.1(4) . . ?
N4 C44 H44A 117.5 . . ?
C43 C44 H44A 117.5 . . ?
C61 C60 N6 123.6(4) . . ?
C61 C60 H60A 118.2 . . ?
N6 C60 H60A 118.2 . . ?
C60 C61 C62 118.8(4) . . ?
C60 C61 H61A 120.6 . . ?
C62 C61 H61A 120.6 . . ?
C63 C62 C61 119.6(4) . . ?
C63 C62 H62A 120.2 . . ?
C61 C62 H62A 120.2 . . ?
C62 C63 C64 120.1(4) . . ?
C62 C63 H63A 119.9 . . ?
C64 C63 H63A 119.9 . . ?
N5 C64 N6 114.7(4) . . ?
N5 C64 C63 125.3(4) . . ?
N6 C64 C63 119.8(4) . . ?
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
W1 N2 2.154(4) 2_656 ?
W1 N2 2.154(3) . ?
W1 N6 2.155(4) . ?
W1 N6 2.155(4) 2_656 ?
W1A N5 2.138(4) 2_656 ?
W1A N5 2.138(4) . ?
W1A N1 2.156(4) . ?
W1A N1 2.156(4) 2_656 ?
N1 C10 1.355(5) . ?
N1 C14 1.379(5) . ?
N2 C14 1.365(5) . ?
N2 C30 1.387(5) . ?
N3 C34 1.333(5) . ?
N3 C30 1.348(5) . ?
N4 C44 1.343(6) . ?
N4 C40 1.350(5) . ?
N5 C64 1.355(5) . ?
N5 C40 1.399(5) . ?
N6 C60 1.369(5) . ?
N6 C64 1.381(5) . ?
C10 C11 1.367(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.395(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.365(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.415(6) . ?
C13 H13A 0.9500 . ?
C30 C31 1.412(6) . ?
C31 C32 1.380(6) . ?
C31 H31A 0.9500 . ?
C32 C33 1.383(7) . ?
C32 H32A 0.9500 . ?
C33 C34 1.369(7) . ?
C33 H33A 0.9500 . ?
C34 H34A 0.9500 . ?
C40 C41 1.399(6) . ?
C41 C42 1.369(6) . ?
C41 H41A 0.9500 . ?
C42 C43 1.386(6) . ?
C42 H42A 0.9500 . ?
C43 C44 1.373(7) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C60 C61 1.358(6) . ?
C60 H60A 0.9500 . ?
C61 C62 1.399(6) . ?
C61 H61A 0.9500 . ?
C62 C63 1.365(6) . ?
C62 H62A 0.9500 . ?
C63 C64 1.420(6) . ?
C63 H63A 0.9500 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N5 W1A N1 C10 93.3(3) 2_656 . . . ?
N5 W1A N1 C10 -82.1(3) . . . . ?
N1 W1A N1 C10 5.5(3) 2_656 . . . ?
N5 W1A N1 C14 -82.9(3) 2_656 . . . ?
N5 W1A N1 C14 101.7(3) . . . . ?
N1 W1A N1 C14 -170.7(3) 2_656 . . . ?
N2 W1 N2 C14 178.3(3) 2_656 . . . ?
N6 W1 N2 C14 -93.9(3) . . . . ?
N6 W1 N2 C14 90.3(3) 2_656 . . . ?
N2 W1 N2 C30 -0.8(3) 2_656 . . . ?
N6 W1 N2 C30 87.1(3) . . . . ?
N6 W1 N2 C30 -88.7(3) 2_656 . . . ?
N5 W1A N5 C64 -173.7(3) 2_656 . . . ?
N1 W1A N5 C64 -86.8(3) . . . . ?
N1 W1A N5 C64 99.2(3) 2_656 . . . ?
N5 W1A N5 C40 12.0(3) 2_656 . . . ?
N1 W1A N5 C40 98.9(3) . . . . ?
N1 W1A N5 C40 -75.1(3) 2_656 . . . ?
N2 W1 N6 C60 94.2(3) 2_656 . . . ?
N2 W1 N6 C60 -83.2(3) . . . . ?
N6 W1 N6 C60 5.5(3) 2_656 . . . ?
N2 W1 N6 C64 -87.8(3) 2_656 . . . ?
N2 W1 N6 C64 94.8(3) . . . . ?
N6 W1 N6 C64 -176.6(3) 2_656 . . . ?
C14 N1 C10 C11 3.6(6) . . . . ?
W1A N1 C10 C11 -172.6(3) . . . . ?
N1 C10 C11 C12 4.8(6) . . . . ?
C10 C11 C12 C13 -6.2(6) . . . . ?
C11 C12 C13 C14 -0.5(6) . . . . ?
C30 N2 C14 N1 -172.5(4) . . . . ?
W1 N2 C14 N1 8.6(5) . . . . ?
C30 N2 C14 C13 10.0(7) . . . . ?
W1 N2 C14 C13 -168.9(3) . . . . ?
C10 N1 C14 N2 172.0(4) . . . . ?
W1A N1 C14 N2 -11.7(5) . . . . ?
C10 N1 C14 C13 -10.3(6) . . . . ?
W1A N1 C14 C13 166.0(3) . . . . ?
C12 C13 C14 N2 -173.7(4) . . . . ?
C12 C13 C14 N1 8.9(6) . . . . ?
C34 N3 C30 N2 -179.2(4) . . . . ?
C34 N3 C30 C31 -3.3(6) . . . . ?
C14 N2 C30 N3 -167.0(4) . . . . ?
W1 N2 C30 N3 12.0(4) . . . . ?
C14 N2 C30 C31 17.6(7) . . . . ?
W1 N2 C30 C31 -163.4(4) . . . . ?
N3 C30 C31 C32 4.0(6) . . . . ?
N2 C30 C31 C32 178.9(4) . . . . ?
C30 C31 C32 C33 -0.9(7) . . . . ?
C31 C32 C33 C34 -2.5(7) . . . . ?
C30 N3 C34 C33 -0.4(7) . . . . ?
C32 C33 C34 N3 3.4(7) . . . . ?
C44 N4 C40 N5 176.1(4) . . . . ?
C44 N4 C40 C41 1.4(6) . . . . ?
C64 N5 C40 N4 145.6(4) . . . . ?
W1A N5 C40 N4 -40.2(4) . . . . ?
C64 N5 C40 C41 -39.8(6) . . . . ?
W1A N5 C40 C41 134.3(4) . . . . ?
N4 C40 C41 C42 -0.3(6) . . . . ?
N5 C40 C41 C42 -174.4(4) . . . . ?
C40 C41 C42 C43 -1.2(6) . . . . ?
C41 C42 C43 C44 1.4(6) . . . . ?
C40 N4 C44 C43 -1.1(7) . . . . ?
C42 C43 C44 N4 -0.3(7) . . . . ?
C64 N6 C60 C61 -1.8(6) . . . . ?
W1 N6 C60 C61 176.2(3) . . . . ?
N6 C60 C61 C62 -1.3(7) . . . . ?
C60 C61 C62 C63 2.4(7) . . . . ?
C61 C62 C63 C64 -0.5(7) . . . . ?
C40 N5 C64 N6 169.2(4) . . . . ?
W1A N5 C64 N6 -4.7(5) . . . . ?
C40 N5 C64 C63 -16.4(7) . . . . ?
W1A N5 C64 C63 169.7(3) . . . . ?
C60 N6 C64 N5 178.5(4) . . . . ?
W1 N6 C64 N5 0.4(5) . . . . ?
C60 N6 C64 C63 3.8(6) . . . . ?
W1 N6 C64 C63 -174.3(3) . . . . ?
C62 C63 C64 N5 -176.8(4) . . . . ?
C62 C63 C64 N6 -2.7(6) . . . . ?
