#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:52:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179310 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/07/4320728.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_4320728
loop_
_publ_author_name
'Sean B. Seymore'
'Seth N. Brown'
_publ_section_title
;
 Synthesis and Cleavage Reactions of Metal-Metal-Bonded
 [Mo2(S2CNR2)6](OTf)2, a Source of the Tris(dithiocarbamato)molybdenum(IV)
 Fragment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6676
_journal_page_last               6683
_journal_paper_doi               10.1021/ic010673y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C14 H16 Cu N5 O S2'
_chemical_formula_weight         397.98
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3436(8)
_cell_length_b                   9.4433(10)
_cell_length_c                   22.347(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1760.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4360
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.487
_exptl_absorpt_correction_T_max  0.8077
_exptl_absorpt_correction_T_min  0.7075
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0293
_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)+(0.0419P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                2614
_reflns_number_total             2916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010673y.cif
_cod_data_source_block           001024a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320728
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
Cu1 Cu 0.15457(5) -0.05125(4) 0.957174(17) 0.04072(12) Uani 1 1 d . . .
S1 S -0.02206(16) -0.24008(11) 0.89727(5) 0.0642(3) Uani 1 1 d . . .
C1 C -0.1402(5) -0.2919(3) 0.95083(15) 0.0487(9) Uani 1 1 d . . .
N1 N -0.2240(5) -0.3293(4) 0.98828(15) 0.0650(10) Uani 1 1 d . . .
S2 S -0.07395(18) 0.09398(15) 1.13623(5) 0.0833(4) Uani 1 1 d . . .
C2 C -0.0160(4) 0.0450(4) 1.07066(15) 0.0465(8) Uani 1 1 d . . .
N2 N 0.0260(4) 0.0120(3) 1.02387(13) 0.0601(9) Uani 1 1 d . . .
C11 C 0.4397(5) -0.1702(4) 0.89119(16) 0.0521(9) Uani 1 1 d . . .
H11A H 0.4524 -0.2295 0.9241 0.063 Uiso 1 1 calc R . .
C12 C 0.5427(5) -0.1849(4) 0.84286(17) 0.0556(10) Uani 1 1 d . . .
H12A H 0.6226 -0.2536 0.8431 0.067 Uiso 1 1 calc R . .
C13 C 0.5247(5) -0.0965(4) 0.79473(15) 0.0516(9) Uani 1 1 d . . .
H13A H 0.5933 -0.1039 0.7621 0.062 Uiso 1 1 calc R . .
C14 C 0.4045(5) 0.0037(4) 0.79489(14) 0.0444(8) Uani 1 1 d . . .
H14A H 0.3906 0.0641 0.7624 0.053 Uiso 1 1 calc R . .
C15 C 0.3050(4) 0.0128(3) 0.84417(14) 0.0349(7) Uani 1 1 d . . .
C16 C 0.1668(4) 0.1056(3) 0.85187(13) 0.0342(7) Uani 1 1 d . . .
C17 C -0.0539(4) 0.2497(3) 0.82872(15) 0.0418(8) Uani 1 1 d . . .
C18 C -0.1714(6) 0.1678(5) 0.79032(18) 0.0642(11) Uani 1 1 d . . .
H18A H -0.1642 0.2001 0.7497 0.096 Uiso 1 1 calc R . .
H18B H -0.2783 0.1827 0.8049 0.096 Uiso 1 1 calc R . .
H18C H -0.1462 0.0687 0.7920 0.096 Uiso 1 1 calc R . .
C19 C -0.0701(6) 0.4085(4) 0.81693(19) 0.0665(12) Uani 1 1 d . . .
H19A H -0.0687 0.4255 0.7746 0.100 Uiso 1 1 calc R . .
H19B H 0.0176 0.4577 0.8354 0.100 Uiso 1 1 calc R . .
H19C H -0.1694 0.4420 0.8334 0.100 Uiso 1 1 calc R . .
C20 C -0.0539(4) 0.2042(3) 0.89705(15) 0.0419(8) Uani 1 1 d . . .
C21 C -0.2105(5) 0.1370(5) 0.91722(19) 0.0642(12) Uani 1 1 d . . .
H21A H -0.2035 0.1129 0.9589 0.096 Uiso 1 1 calc R . .
H21B H -0.2302 0.0529 0.8942 0.096 Uiso 1 1 calc R . .
H21C H -0.2968 0.2027 0.9113 0.096 Uiso 1 1 calc R . .
C22 C -0.0064(6) 0.3245(3) 0.93908(17) 0.0644(12) Uani 1 1 d . . .
H22A H -0.0091 0.2915 0.9797 0.097 Uiso 1 1 calc R . .
H22B H -0.0801 0.4018 0.9345 0.097 Uiso 1 1 calc R . .
H22C H 0.1000 0.3560 0.9295 0.097 Uiso 1 1 calc R . .
N3 N 0.3236(4) -0.0741(3) 0.89194(11) 0.0406(6) Uani 1 1 d . . .
N4 N 0.0794(3) 0.0982(2) 0.89926(11) 0.0340(6) Uani 1 1 d . . .
N5 N 0.1085(3) 0.2009(3) 0.81053(12) 0.0401(7) Uani 1 1 d . . .
O1 O 0.1741(4) 0.2330(3) 0.76124(10) 0.0564(7) 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 0.0033 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cu1 N1 89.15(14) . 4_547 ?
N2 Cu1 N4 96.08(12) . . ?
N1 Cu1 N4 166.08(14) 4_547 . ?
N2 Cu1 N3 165.55(13) . . ?
N1 Cu1 N3 91.51(13) 4_547 . ?
N4 Cu1 N3 80.23(10) . . ?
N2 Cu1 S1 106.66(12) . . ?
N1 Cu1 S1 102.36(12) 4_547 . ?
N4 Cu1 S1 88.52(8) . . ?
N3 Cu1 S1 87.29(8) . . ?
C1 S1 Cu1 99.60(13) . . ?
N1 C1 S1 179.5(4) . . ?
C1 N1 Cu1 162.5(3) . 4_447 ?
N2 C2 S2 179.0(4) . . ?
C2 N2 Cu1 163.4(3) . . ?
N3 C11 C12 122.0(3) . . ?
C13 C12 C11 118.8(4) . . ?
C12 C13 C14 119.8(3) . . ?
C13 C14 C15 118.8(3) . . ?
N3 C15 C14 121.4(3) . . ?
N3 C15 C16 111.2(3) . . ?
C14 C15 C16 127.3(3) . . ?
N4 C16 N5 112.8(3) . . ?
N4 C16 C15 120.8(3) . . ?
N5 C16 C15 126.3(3) . . ?
N5 C17 C18 106.0(3) . . ?
N5 C17 C19 109.7(3) . . ?
C18 C17 C19 110.2(3) . . ?
N5 C17 C20 100.3(2) . . ?
C18 C17 C20 114.0(3) . . ?
C19 C17 C20 115.6(3) . . ?
N4 C20 C21 110.4(3) . . ?
N4 C20 C22 106.5(3) . . ?
C21 C20 C22 110.6(3) . . ?
N4 C20 C17 102.3(2) . . ?
C21 C20 C17 113.4(3) . . ?
C22 C20 C17 113.0(3) . . ?
C11 N3 C15 119.2(3) . . ?
C11 N3 Cu1 125.9(2) . . ?
C15 N3 Cu1 114.8(2) . . ?
C16 N4 C20 110.9(3) . . ?
C16 N4 Cu1 112.9(2) . . ?
C20 N4 Cu1 136.1(2) . . ?
O1 N5 C16 125.9(3) . . ?
O1 N5 C17 123.8(3) . . ?
C16 N5 C17 109.9(3) . . ?
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
Cu1 N2 1.931(3) . ?
Cu1 N1 1.946(3) 4_547 ?
Cu1 N4 2.015(2) . ?
Cu1 N3 2.040(3) . ?
Cu1 S1 2.6728(11) . ?
S1 C1 1.626(4) . ?
C1 N1 1.146(5) . ?
N1 Cu1 1.946(3) 4_447 ?
S2 C2 1.611(4) . ?
C2 N2 1.146(4) . ?
C11 N3 1.328(4) . ?
C11 C12 1.387(5) . ?
C12 C13 1.370(5) . ?
C13 C14 1.379(5) . ?
C14 C15 1.381(5) . ?
C15 N3 1.355(4) . ?
C15 C16 1.459(5) . ?
C16 N4 1.287(4) . ?
C16 N5 1.379(4) . ?
C17 N5 1.488(4) . ?
C17 C18 1.515(5) . ?
C17 C19 1.528(4) . ?
C17 C20 1.586(5) . ?
C20 N4 1.497(4) . ?
C20 C21 1.521(5) . ?
C20 C22 1.526(5) . ?
N5 O1 1.267(3) . ?
