#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:55:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180240 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/26/7112679.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_7112679
loop_
_publ_author_name
'Tan, Ai Ling'
'Blake, Alexander J.'
'Davies, E. Stephen'
'Wilson, Claire'
'Garner, C. David'
_publ_section_title
;
 A radical pathway to synthesise Mo and W dithiolene complexes.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              953
_journal_page_last               954
_journal_paper_doi               10.1039/c0cc03756g
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C25 H25 Mo N S2'
_chemical_formula_sum            'C25 H25 Mo N S2'
_chemical_formula_weight         499.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.509(5)
_cell_length_b                   15.496(7)
_cell_length_c                   12.056(5)
_cell_measurement_reflns_used    2920
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52.6
_cell_measurement_theta_min      4.4
_cell_volume                     2150.1(16)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    ' ? '
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_av_sigmaI/netI    0.017
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6628
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS version 2.05; Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.58
_refine_diff_density_rms         0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.54(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.038P)²+12.212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.100
_reflns_number_gt                2246
_reflns_number_total             2532
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c0cc03756g.txt
_cod_data_source_block           cpmohx
_cod_original_cell_volume        2150(3)
_cod_database_code               7112679
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, 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'
'-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
Mo1 Mo 1.0000 -0.01890(3) 0.2214(3) 0.02956(13) Uani 1 2 d S . .
C1A C 0.8662 -0.11098(3) 0.1183(3) 0.027(3) Uiso 0.367(18) 1 d PRD A 1
H1AA H 0.8854 -0.1453 0.0505 0.032 Uiso 0.367(18) 1 calc PR A 1
C2A C 0.8194 -0.02619(3) 0.1199(3) 0.033(4) Uiso 0.367(18) 1 d PRD A 1
H2AA H 0.7985 0.0092 0.0535 0.039 Uiso 0.367(18) 1 calc PR A 1
C3A C 0.8043 -0.00152(3) 0.2324(3) 0.039(4) Uiso 0.367(18) 1 d PRD A 1
H3AA H 0.7633 0.0515 0.2589 0.047 Uiso 0.367(18) 1 calc PR A 1
C4A C 0.8417 -0.07106(3) 0.3003(3) 0.044(5) Uiso 0.367(18) 1 d PRD A 1
H4AA H 0.8283 -0.0761 0.3820 0.052 Uiso 0.367(18) 1 calc PR A 1
C5A C 0.8800 -0.13871(3) 0.2297(3) 0.039(3) Uiso 0.367(18) 1 d PRD A 1
H5AA H 0.9036 -0.1979 0.2541 0.047 Uiso 0.367(18) 1 calc PR A 1
C1B C 0.8782(8) -0.1358(5) 0.1793(9) 0.053(3) Uiso 0.633(18) 1 d PD A 2
H1BA H 0.9033 -0.1929 0.1492 0.064 Uiso 0.633(18) 1 calc PR A 2
C2B C 0.8433(7) -0.0651(5) 0.1176(8) 0.042(2) Uiso 0.633(18) 1 d PD A 2
H2BA H 0.8390 -0.0634 0.0348 0.051 Uiso 0.633(18) 1 calc PR A 2
C3B C 0.7982(9) -0.0028(6) 0.1875(8) 0.060(3) Uiso 0.633(18) 1 d PD A 2
H3BA H 0.7584 0.0516 0.1638 0.072 Uiso 0.633(18) 1 calc PR A 2
C4B C 0.8081(7) -0.0331(4) 0.2966(7) 0.034(2) Uiso 0.633(18) 1 d PD A 2
H4BA H 0.7782 -0.0031 0.3643 0.041 Uiso 0.633(18) 1 calc PR A 2
C5B C 0.8641(7) -0.1141(4) 0.2947(8) 0.037(2) Uiso 0.633(18) 1 d PD A 2
H5BA H 0.8758 -0.1537 0.3593 0.044 Uiso 0.633(18) 1 calc PR A 2
S1 S 1.0000 0.0998(2) 0.3512(4) 0.0460(9) Uani 1 2 d S . .
S2 S 1.0000 0.0983(2) 0.0897(3) 0.0438(9) Uani 1 2 d S . .
C1 C 1.0000 0.3710(10) 0.5597(10) 0.071(5) Uani 1 2 d S . .
H1A H 1.0000 0.3242 0.6157 0.085 Uiso 1 2 calc SR . .
H1B H 1.0000 0.4268 0.5996 0.085 Uiso 1 2 calc SR . .
C4 C 1.0000 0.2836(8) 0.3394(13) 0.060(3) Uani 1 2 d S . .
C5 C 1.0000 0.1954(6) 0.2749(12) 0.050(4) Uani 1 2 d S . .
C6 C 1.0000 0.1995(7) 0.1639(9) 0.041(3) Uiso 1 2 d SD . .
C7 C 1.0000 0.2626(6) 0.0736(7) 0.063(4) Uani 1 2 d SD . .
C8 C 0.8931(8) 0.2902(4) 0.4131(7) 0.043(2) Uani 1 1 d . . .
H8A H 0.8235 0.2970 0.3657 0.051 Uiso 1 1 calc R . .
H8B H 0.8844 0.2357 0.4552 0.051 Uiso 1 1 calc R . .
C9 C 0.8989(11) 0.3647(7) 0.4937(8) 0.068(3) Uani 1 1 d . . .
H9A H 0.8909 0.4189 0.4510 0.081 Uiso 1 1 calc R . .
H9B H 0.8309 0.3607 0.5438 0.081 Uiso 1 1 calc R . .
C10 C 1.0000 0.3645(5) 0.2621(6) 0.0424(16) Uani 1 2 d S . .
C13 C 1.0000 0.3823(8) -0.0997(10) 0.064(4) Uani 1 2 d SD . .
H13A H 1.0000 0.4215 -0.1603 0.077 Uiso 1 2 calc SR . .
C14 C 1.1115(11) 0.3534(7) -0.0550(8) 0.069(3) Uani 1 1 d D . .
H14A H 1.1833 0.3748 -0.0825 0.082 Uiso 1 1 calc R . .
C15 C 1.1065(9) 0.2934(6) 0.0293(7) 0.054(3) Uani 1 1 d D . .
H15A H 1.1773 0.2717 0.0589 0.065 Uiso 1 1 calc R . .
N1 N 1.0000 0.4317(4) 0.2125(10) 0.0555(18) Uani 1 2 d S . .
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'
S S 0.1246 0.1234 '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
C5A C1A C2A 108.0 . .
C3A C2A C1A 108.0 . .
C2A C3A C4A 108.0 . .
C3A C4A C5A 108.0 . .
C1A C5A C4A 108.0 . .
C2B C1B C5B 107.6(7) . .
C3B C2B C1B 109.5(7) . .
C2B C3B C4B 107.9(7) . .
C3B C4B C5B 108.7(7) . .
C4B C5B C1B 105.9(7) . .
C5 S1 Mo1 107.8(5) . .
C6 S2 Mo1 109.2(4) . .
C5 C6 C7 140.8(10) . .
C5 C6 S2 117.0(11) . .
C7 C6 S2 102.2(5) . .
C15 C7 C15 119.5(14) 3_755 .
C15 C7 C6 120.3(7) 3_755 .
C15 C7 C6 120.3(7) . .
C14 C13 C14 122.8(12) . 3_755
C15 C14 C13 116.2(10) . .
C14 C15 C7 122.6(11) . .
C8 C4 C8 108.0(12) 3_755 .
C8 C4 C10 107.2(6) 3_755 .
C8 C4 C10 107.2(6) . .
C8 C4 C5 110.3(7) 3_755 .
C8 C4 C5 110.3(7) . .
C10 C4 C5 113.7(11) . .
C6 C5 C4 116.9(12) . .
C6 C5 S1 124.5(10) . .
C4 C5 S1 118.5(10) . .
C9 C8 C4 113.0(8) . .
C1 C9 C8 116.8(10) . .
C9 C1 C9 110.8(11) . 3_755
N1 C10 C4 173.3(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mo1 C4A 2.2084
Mo1 C3A 2.2724
Mo1 C2B 2.309(8)
Mo1 C5A 2.3164
Mo1 C5B 2.325(8)
Mo1 C1B 2.346(10)
C1A C5A 1.4199
C1A C2A 1.4200
C2A C3A 1.4200
C3A C4A 1.4200
C4A C5A 1.4201
C1B C2B 1.383(8)
C1B C5B 1.440(8)
C2B C3B 1.382(8)
C3B C4B 1.401(8)
C4B C5B 1.412(7)
S1 C5 1.745(14)
S2 C6 1.805(11)
C6 C5 1.339(10)
C6 C7 1.464(18)
C7 C15 1.420(11)
C13 C14 1.462(13)
C14 C15 1.379(15)
C4 C8 1.520(12)
C4 C10 1.561(17)
C4 C5 1.573(15)
C8 C9 1.511(12)
C9 C1 1.414(14)
N1 C10 1.202(11)
