#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:15:37 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230427 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/70/7057092.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_7057092
loop_
_publ_author_name
'Bose, Moumita'
'Moula, Golam'
'Begum, Ameerunisha'
'Sarkar, Sabyasachi'
_publ_section_title
;
 Synthesis and characterization of cyano and isocyano complexes of
 bis(dithiolato) molybdenum using Me3SiCN: a route to a cyanide-bridged
 multimer to a monomer
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5580
_journal_paper_doi               10.1039/C8NJ00246K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C16 H18 Mo N6 S4 Si2'
_chemical_formula_sum            'C16 H18 Mo N6 S4 Si2'
_chemical_formula_weight         574.72
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_audit_update_record
;
2012-11-25 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 120.919(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   20.059(5)
_cell_length_b                   9.487(5)
_cell_length_c                   15.979(5)
_cell_measurement_temperature    100(2)
_cell_volume                     2608.7(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7647
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.821
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.498
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.498
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0600
_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)+(0.1130P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.2479
_reflns_number_gt                2150
_reflns_number_total             2832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8nj00246k2.cif
_cod_data_source_block           22junc
_cod_depositor_comments
'Adding full bibliography for 7057091--7057093.cif.'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7057092
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
C1 C 0.6458(4) 0.2077(7) 0.5583(5) 0.0267(15) Uani 1 1 d .
C2 C 0.5845(4) 0.1505(7) 0.4677(5) 0.0260(14) Uani 1 1 d .
C3 C 0.5092(4) 0.1573(7) 0.4409(5) 0.0293(15) Uani 1 1 d .
C4 C 0.4841(4) 0.2237(7) 0.4998(5) 0.0250(14) Uani 1 1 d .
C5 C 0.4258(4) -0.1710(7) 0.2225(5) 0.0237(14) Uani 1 1 d .
C6 C 0.3680(5) -0.5285(8) 0.2868(6) 0.0391(19) Uani 1 1 d .
H6A H 0.4234 -0.5349 0.3167 0.059 Uiso 1 1 calc R
H6B H 0.3460 -0.6215 0.2722 0.059 Uiso 1 1 calc R
H6C H 0.3556 -0.4828 0.3307 0.059 Uiso 1 1 calc R
C7 C 0.2291(4) -0.3561(8) 0.1259(5) 0.0336(17) Uani 1 1 d .
H7A H 0.2293 -0.2903 0.1717 0.050 Uiso 1 1 calc R
H7B H 0.1942 -0.4322 0.1159 0.050 Uiso 1 1 calc R
H7C H 0.2122 -0.3092 0.0650 0.050 Uiso 1 1 calc R
C8 C 0.3411(5) -0.5151(8) 0.0808(7) 0.042(2) Uani 1 1 d .
H8A H 0.3223 -0.4552 0.0247 0.063 Uiso 1 1 calc R
H8B H 0.3126 -0.6021 0.0622 0.063 Uiso 1 1 calc R
H8C H 0.3953 -0.5343 0.1071 0.063 Uiso 1 1 calc R
N1 N 0.6969(4) 0.2505(7) 0.6306(5) 0.0440(17) Uani 1 1 d .
N2 N 0.4640(4) 0.2803(7) 0.5485(5) 0.0394(15) Uani 1 1 d .
N3 N 0.3879(3) -0.2691(6) 0.2066(4) 0.0291(13) Uani 1 1 d .
Si1 Si 0.32797(12) -0.42636(19) 0.17412(15) 0.0272(5) Uani 1 1 d .
S1 S 0.61302(10) 0.07790(17) 0.39228(13) 0.0254(4) Uani 1 1 d .
S2 S 0.43875(10) 0.08324(16) 0.33251(12) 0.0238(4) Uani 1 1 d .
Mo1 Mo 0.5000 0.00100(7) 0.2500 0.0205(3) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.030(4) 0.029(3) 0.017(3) -0.005(3) 0.009(3) 0.008(3)
C2 0.026(3) 0.026(3) 0.026(4) 0.005(3) 0.014(3) 0.000(3)
C3 0.040(4) 0.022(3) 0.032(4) 0.003(3) 0.022(3) 0.006(3)
C4 0.028(3) 0.028(3) 0.018(3) 0.004(3) 0.012(3) -0.003(3)
C5 0.023(3) 0.022(3) 0.030(4) -0.020(3) 0.017(3) -0.011(3)
C6 0.040(5) 0.025(3) 0.045(5) -0.001(3) 0.017(4) -0.003(3)
C7 0.021(3) 0.040(4) 0.031(4) -0.013(3) 0.007(3) -0.008(3)
C8 0.040(5) 0.043(5) 0.058(6) -0.008(4) 0.036(5) -0.002(4)
N1 0.044(4) 0.044(4) 0.039(4) 0.003(3) 0.018(3) 0.009(3)
N2 0.040(4) 0.052(4) 0.031(4) 0.003(3) 0.021(3) -0.002(3)
N3 0.030(3) 0.030(3) 0.023(3) 0.000(3) 0.011(3) 0.006(3)
Si1 0.0288(11) 0.0224(9) 0.0331(11) -0.0002(8) 0.0179(9) -0.0007(8)
S1 0.0237(9) 0.0276(9) 0.0240(9) -0.0010(7) 0.0117(7) 0.0012(7)
S2 0.0229(9) 0.0254(8) 0.0254(9) -0.0011(7) 0.0141(7) -0.0014(6)
Mo1 0.0213(5) 0.0192(5) 0.0216(5) 0.000 0.0115(4) 0.000
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'
Si Si 0.0817 0.0704 '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
N1 C1 C2 177.5(7) . .
C3 C2 C1 122.8(6) . .
C3 C2 S1 121.3(6) . .
C1 C2 S1 115.8(5) . .
C2 C3 C4 122.2(7) . .
C2 C3 S2 120.5(5) . .
C4 C3 S2 117.3(5) . .
N2 C4 C3 179.0(8) . .
N3 C5 Mo1 176.4(5) . .
Si1 C6 H6A 109.5 . .
Si1 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
Si1 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si1 C7 H7A 109.5 . .
Si1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
Si1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
Si1 C8 H8A 109.5 . .
Si1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
Si1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C5 N3 Si1 176.1(6) . .
N3 Si1 C6 105.2(3) . .
N3 Si1 C7 103.5(3) . .
C6 Si1 C7 115.9(4) . .
N3 Si1 C8 104.9(3) . .
C6 Si1 C8 112.4(4) . .
C7 Si1 C8 113.4(4) . .
C2 S1 Mo1 107.4(2) . .
C3 S2 Mo1 107.7(2) . .
C5 Mo1 C5 77.8(3) . 2_655
C5 Mo1 S2 131.29(17) . 2_655
C5 Mo1 S2 81.77(17) 2_655 2_655
C5 Mo1 S2 81.77(17) . .
C5 Mo1 S2 131.29(17) 2_655 .
S2 Mo1 S2 141.22(8) 2_655 .
C5 Mo1 S1 132.1(2) . .
C5 Mo1 S1 79.1(2) 2_655 .
S2 Mo1 S1 85.26(6) 2_655 .
S2 Mo1 S1 82.93(6) . .
C5 Mo1 S1 79.1(2) . 2_655
C5 Mo1 S1 132.1(2) 2_655 2_655
S2 Mo1 S1 82.93(6) 2_655 2_655
S2 Mo1 S1 85.26(6) . 2_655
S1 Mo1 S1 143.90(9) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.155(9) .
C1 C2 1.439(9) .
C2 C3 1.344(10) .
C2 S1 1.721(7) .
C3 C4 1.422(10) .
C3 S2 1.724(8) .
C4 N2 1.174(9) .
C5 N3 1.145(8) .
C5 Mo1 2.097(6) .
C6 Si1 1.828(8) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 Si1 1.845(7) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 Si1 1.845(8) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
N3 Si1 1.816(6) .
S1 Mo1 2.3545(18) .
S2 Mo1 2.3497(17) .
Mo1 C5 2.097(6) 2_655
Mo1 S2 2.3497(17) 2_655
Mo1 S1 2.3545(18) 2_655
