#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:50:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180157 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/53/7105360.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_7105360
loop_
_publ_author_name
'Brown, Neil J'
'Collison, David'
'Edge, Ruth'
'Fitzgerald, Emma C'
'Low, Paul J'
'Helliwell, Madeleine'
'Ta, Yien T'
'Whiteley, Mark W'
_publ_section_title
;
 Metal-stabilised diynyl radicals: structure and reactivity of
 [Mo(C[triple bond]C-C[triple bond]CSiMe3)L2(eta-C7H7)]*+ (L2 =
 2,2'-bipyridine or dppe).
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2253
_journal_page_last               2255
_journal_paper_doi               10.1039/b924759a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C24 H24 F6 Mo N2 P Si'
_chemical_formula_weight         609.45
_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                111.281(5)
_cell_angle_beta                 96.047(5)
_cell_angle_gamma                105.029(5)
_cell_formula_units_Z            2
_cell_length_a                   8.068(5)
_cell_length_b                   12.306(5)
_cell_length_c                   14.276(5)
_cell_measurement_reflns_used    370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.55
_cell_measurement_theta_min      2.68
_cell_volume                     1243.8(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2478
_diffrn_reflns_av_sigmaI/netI    0.3437
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3696
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.612
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.1824
_refine_ls_R_factor_gt           0.0927
_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)+(0.0712P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2219
_reflns_number_gt                1077
_reflns_number_total             2538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924759a.txt
_cod_data_source_block           s2133m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105360
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.2345(2) 0.08896(19) 0.22868(15) 0.0269(6) Uani 1 1 d U . .
Si1 Si 0.4817(8) 0.3287(6) -0.1819(5) 0.0414(17) Uani 1 1 d U . .
N1 N 0.0422(18) 0.1819(15) 0.2132(12) 0.025(2) Uani 1 1 d U . .
N2 N 0.3770(18) 0.2814(14) 0.3132(11) 0.027(2) Uani 1 1 d U . .
C1 C 0.413(3) 0.0502(19) 0.3368(16) 0.042(2) Uani 1 1 d U . .
H1 H 0.5164 0.0941 0.3875 0.050 Uiso 1 1 calc R . .
C2 C 0.242(3) 0.0477(19) 0.3709(17) 0.040(2) Uani 1 1 d U . .
H2 H 0.2536 0.0929 0.4408 0.048 Uiso 1 1 calc R . .
C3 C 0.081(3) -0.0074(18) 0.3183(16) 0.040(2) Uani 1 1 d U . .
H3 H -0.0079 -0.0018 0.3544 0.049 Uiso 1 1 calc R . .
C4 C 0.028(3) -0.0780(18) 0.2061(16) 0.041(2) Uani 1 1 d U . .
H4 H -0.0931 -0.1051 0.1803 0.050 Uiso 1 1 calc R . .
C5 C 0.123(3) -0.1122(19) 0.1309(18) 0.045(3) Uani 1 1 d U . .
H5 H 0.0615 -0.1606 0.0631 0.053 Uiso 1 1 calc R . .
C6 C 0.300(3) -0.0787(19) 0.1510(17) 0.046(3) Uani 1 1 d U . .
H6 H 0.3443 -0.1121 0.0932 0.056 Uiso 1 1 calc R . .
C7 C 0.430(3) -0.0057(19) 0.2388(17) 0.044(2) Uani 1 1 d U . .
H7 H 0.5450 0.0070 0.2298 0.052 Uiso 1 1 calc R . .
C8 C 0.300(2) 0.1319(18) 0.1045(15) 0.026(2) Uani 1 1 d U . .
C9 C 0.338(2) 0.1733(17) 0.0396(14) 0.025(2) Uani 1 1 d U . .
C10 C 0.392(2) 0.2229(18) -0.0267(15) 0.027(3) Uani 1 1 d U . .
C11 C 0.415(2) 0.2568(18) -0.0947(15) 0.030(3) Uani 1 1 d U . .
C12 C 0.398(3) 0.211(2) -0.3140(14) 0.052(6) Uani 1 1 d U . .
H12A H 0.4579 0.2393 -0.3596 0.078 Uiso 1 1 calc R . .
H12B H 0.2742 0.1954 -0.3343 0.078 Uiso 1 1 calc R . .
H12C H 0.4189 0.1364 -0.3173 0.078 Uiso 1 1 calc R . .
C13 C 0.718(3) 0.390(2) -0.1542(18) 0.068(7) Uani 1 1 d U . .
H13A H 0.7670 0.3254 -0.1621 0.102 Uiso 1 1 calc R . .
H13B H 0.7595 0.4517 -0.0847 0.102 Uiso 1 1 calc R . .
H13C H 0.7523 0.4271 -0.2010 0.102 Uiso 1 1 calc R . .
C14 C 0.378(3) 0.4497(19) -0.1584(17) 0.055(6) Uani 1 1 d U . .
H14A H 0.4599 0.5267 -0.1093 0.082 Uiso 1 1 calc R . .
H14B H 0.2755 0.4288 -0.1317 0.082 Uiso 1 1 calc R . .
H14C H 0.3442 0.4569 -0.2219 0.082 Uiso 1 1 calc R . .
C15 C -0.120(2) 0.1185(18) 0.1530(14) 0.025(3) Uani 1 1 d U . .
H15 H -0.1512 0.0338 0.1158 0.030 Uiso 1 1 calc R . .
C16 C -0.236(2) 0.1777(18) 0.1468(14) 0.027(3) Uani 1 1 d U . .
H16 H -0.3510 0.1322 0.1096 0.033 Uiso 1 1 calc R . .
C17 C -0.190(2) 0.3016(18) 0.1931(14) 0.027(3) Uani 1 1 d U . .
H17 H -0.2705 0.3414 0.1842 0.033 Uiso 1 1 calc R . .
C18 C -0.020(2) 0.3697(18) 0.2551(14) 0.027(3) Uani 1 1 d U . .
H18 H 0.0155 0.4547 0.2918 0.032 Uiso 1 1 calc R . .
C19 C 0.091(2) 0.3001(18) 0.2573(14) 0.025(2) Uani 1 1 d U . .
C20 C 0.277(2) 0.3630(18) 0.3177(14) 0.026(2) Uani 1 1 d U . .
C21 C 0.352(2) 0.4856(18) 0.3605(14) 0.027(3) Uani 1 1 d U . .
H21 H 0.2827 0.5362 0.3639 0.033 Uiso 1 1 calc R . .
C22 C 0.535(2) 0.5381(19) 0.4005(14) 0.031(3) Uani 1 1 d U . .
H22 H 0.5932 0.6224 0.4262 0.037 Uiso 1 1 calc R . .
C23 C 0.623(2) 0.4537(18) 0.3982(15) 0.031(3) Uani 1 1 d U . .
H23 H 0.7420 0.4837 0.4284 0.037 Uiso 1 1 calc R . .
C24 C 0.546(2) 0.3347(18) 0.3559(14) 0.028(3) Uani 1 1 d U . .
H24 H 0.6144 0.2847 0.3560 0.034 Uiso 1 1 calc R . .
P1 P 0.9164(7) 0.2556(6) 0.5118(5) 0.0385(13) Uani 1 1 d U . .
F1 F 0.9221(13) 0.3837(10) 0.5062(9) 0.046(2) Uani 1 1 d U . .
F2 F 1.0061(15) 0.3311(11) 0.6325(8) 0.054(3) Uani 1 1 d U . .
F3 F 0.7289(13) 0.2422(11) 0.5376(9) 0.050(3) Uani 1 1 d U . .
F4 F 0.9161(14) 0.1323(10) 0.5198(9) 0.053(2) Uani 1 1 d U . .
F5 F 0.8284(13) 0.1830(10) 0.3907(8) 0.045(3) Uani 1 1 d U . .
F6 F 1.1032(12) 0.2699(10) 0.4839(8) 0.042(2) Uani 1 1 d U . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
C8 Mo1 N2 81.4(6) . . ?
C8 Mo1 C4 122.2(7) . . ?
N2 Mo1 C4 151.6(7) . . ?
C8 Mo1 N1 80.9(6) . . ?
N2 Mo1 N1 75.4(6) . . ?
C4 Mo1 N1 91.8(6) . . ?
C8 Mo1 C6 84.8(8) . . ?
N2 Mo1 C6 136.3(7) . . ?
C4 Mo1 C6 67.1(8) . . ?
N1 Mo1 C6 142.4(7) . . ?
C8 Mo1 C7 97.2(8) . . ?
N2 Mo1 C7 105.0(7) . . ?
C4 Mo1 C7 88.8(8) . . ?
N1 Mo1 C7 178.0(8) . . ?
C6 Mo1 C7 36.4(7) . . ?
C8 Mo1 C5 93.2(8) . . ?
N2 Mo1 C5 171.2(7) . . ?
C4 Mo1 C5 36.8(7) . . ?
N1 Mo1 C5 110.7(7) . . ?
C6 Mo1 C5 35.5(7) . . ?
C7 Mo1 C5 68.7(8) . . ?
C8 Mo1 C1 125.6(7) . . ?
N2 Mo1 C1 88.1(7) . . ?
C4 Mo1 C1 89.4(7) . . ?
N1 Mo1 C1 146.7(7) . . ?
C6 Mo1 C1 67.2(7) . . ?
C7 Mo1 C1 35.3(7) . . ?
C5 Mo1 C1 89.5(7) . . ?
C8 Mo1 C2 164.5(6) . . ?
N2 Mo1 C2 94.1(7) . . ?
C4 Mo1 C2 67.1(7) . . ?
N1 Mo1 C2 112.5(6) . . ?
C6 Mo1 C2 88.4(8) . . ?
C7 Mo1 C2 69.5(7) . . ?
C5 Mo1 C2 89.4(8) . . ?
C1 Mo1 C2 39.0(7) . . ?
C8 Mo1 C3 159.8(7) . . ?
N2 Mo1 C3 116.0(7) . . ?
C4 Mo1 C3 38.3(7) . . ?
N1 Mo1 C3 93.1(6) . . ?
C6 Mo1 C3 88.4(8) . . ?
C7 Mo1 C3 88.5(8) . . ?
C5 Mo1 C3 70.8(8) . . ?
C1 Mo1 C3 68.0(7) . . ?
C2 Mo1 C3 33.0(6) . . ?
C13 Si1 C11 109.8(9) . . ?
C13 Si1 C12 110.4(11) . . ?
C11 Si1 C12 108.0(10) . . ?
C13 Si1 C14 112.0(11) . . ?
C11 Si1 C14 105.0(10) . . ?
C12 Si1 C14 111.4(10) . . ?
C19 N1 C15 120.2(15) . . ?
C19 N1 Mo1 118.5(12) . . ?
C15 N1 Mo1 121.2(13) . . ?
C24 N2 C20 115.6(16) . . ?
C24 N2 Mo1 128.7(12) . . ?
C20 N2 Mo1 115.6(11) . . ?
C7 C1 C2 126(2) . . ?
C7 C1 Mo1 70.4(11) . . ?
C2 C1 Mo1 70.6(10) . . ?
C7 C1 H1 117.1 . . ?
C2 C1 H1 117.1 . . ?
Mo1 C1 H1 137.1 . . ?
C3 C2 C1 130(2) . . ?
C3 C2 Mo1 74.7(13) . . ?
C1 C2 Mo1 70.4(11) . . ?
C3 C2 H2 114.9 . . ?
C1 C2 H2 114.9 . . ?
Mo1 C2 H2 135.5 . . ?
C2 C3 C4 125(2) . . ?
C2 C3 Mo1 72.3(13) . . ?
C4 C3 Mo1 66.6(12) . . ?
C2 C3 H3 117.3 . . ?
C4 C3 H3 117.3 . . ?
Mo1 C3 H3 139.7 . . ?
C5 C4 C3 132(2) . . ?
C5 C4 Mo1 73.6(13) . . ?
C3 C4 Mo1 75.1(12) . . ?
C5 C4 H4 113.8 . . ?
C3 C4 H4 113.8 . . ?
Mo1 C4 H4 132.1 . . ?
C6 C5 C4 123(2) . . ?
C6 C5 Mo1 70.8(13) . . ?
C4 C5 Mo1 69.6(12) . . ?
C6 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
Mo1 C5 H5 135.6 . . ?
C5 C6 C7 134(2) . . ?
C5 C6 Mo1 73.6(13) . . ?
C7 C6 Mo1 72.6(12) . . ?
C5 C6 H6 113.2 . . ?
C7 C6 H6 113.2 . . ?
Mo1 C6 H6 137.4 . . ?
C1 C7 C6 129(2) . . ?
C1 C7 Mo1 74.3(11) . . ?
C6 C7 Mo1 71.0(12) . . ?
C1 C7 H7 115.6 . . ?
C6 C7 H7 115.6 . . ?
Mo1 C7 H7 133.7 . . ?
C9 C8 Mo1 171.1(16) . . ?
C8 C9 C10 175.6(18) . . ?
C11 C10 C9 169.9(19) . . ?
C10 C11 Si1 170.2(18) . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 C16 119.8(18) . . ?
N1 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 121.6(18) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C16 C17 C18 119.2(17) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C19 C18 C17 115.0(18) . . ?
C19 C18 H18 122.5 . . ?
C17 C18 H18 122.5 . . ?
N1 C19 C18 123.8(17) . . ?
N1 C19 C20 116.3(15) . . ?
C18 C19 C20 119.8(18) . . ?
C21 C20 N2 122.0(16) . . ?
C21 C20 C19 123.2(16) . . ?
N2 C20 C19 114.1(16) . . ?
C20 C21 C22 120.1(17) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 114.6(18) . . ?
C23 C22 H22 122.7 . . ?
C21 C22 H22 122.7 . . ?
C24 C23 C22 123.5(18) . . ?
C24 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
C23 C24 N2 123.9(17) . . ?
C23 C24 H24 118.0 . . ?
N2 C24 H24 118.0 . . ?
F4 P1 F3 91.6(7) . . ?
F4 P1 F6 89.3(6) . . ?
F3 P1 F6 178.8(8) . . ?
F4 P1 F1 178.3(7) . . ?
F3 P1 F1 89.3(6) . . ?
F6 P1 F1 89.8(6) . . ?
F4 P1 F5 90.6(7) . . ?
F3 P1 F5 90.7(6) . . ?
F6 P1 F5 88.5(6) . . ?
F1 P1 F5 90.8(6) . . ?
F4 P1 F2 90.6(7) . . ?
F3 P1 F2 89.8(7) . . ?
F6 P1 F2 91.0(6) . . ?
F1 P1 F2 87.9(7) . . ?
F5 P1 F2 178.6(8) . . ?
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
Mo1 C8 2.11(2) . ?
Mo1 N2 2.147(16) . ?
Mo1 C4 2.18(2) . ?
Mo1 N1 2.190(14) . ?
Mo1 C6 2.19(2) . ?
Mo1 C7 2.213(18) . ?
Mo1 C5 2.23(2) . ?
Mo1 C1 2.260(18) . ?
Mo1 C2 2.26(2) . ?
Mo1 C3 2.29(2) . ?
Si1 C13 1.80(2) . ?
Si1 C11 1.82(2) . ?
Si1 C12 1.83(2) . ?
Si1 C14 1.837(19) . ?
N1 C19 1.29(2) . ?
N1 C15 1.34(2) . ?
N2 C24 1.31(2) . ?
N2 C20 1.43(2) . ?
C1 C7 1.36(3) . ?
C1 C2 1.51(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.29(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.47(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.39(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.35(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.38(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.24(2) . ?
C9 C10 1.35(2) . ?
C10 C11 1.20(2) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.34(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.35(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.41(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.40(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.49(2) . ?
C20 C21 1.34(2) . ?
C21 C22 1.41(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.39(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.30(2) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
P1 F4 1.561(12) . ?
P1 F3 1.576(12) . ?
P1 F6 1.581(11) . ?
P1 F1 1.597(12) . ?
P1 F5 1.607(12) . ?
P1 F2 1.608(12) . ?
