#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:15:55 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321664.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_4321664
loop_
_publ_author_name
'P. Schollhammer'
'F. Y. Pétillon'
'J. Talarmin'
'K. W. Muir'
'H. K. Fun'
'K. Chinnakali'
_publ_section_title
;
 Halogenation and Alkylation at a MoIII2(μ-S) Site. Crystal Structure of
 the Metal-Sulfenyl Halide Complex
 [Mo2(η5-C5Me5)2(μ-SMe)2(μ-SI)(CO)2]I5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5879
_journal_page_last               5882
_journal_paper_doi               10.1021/ic000591u
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'synthesis by authors'
_chemical_formula_moiety         'C10 H17 Cl4 Mo O'
_chemical_formula_sum            'C10 H17 Cl4 Mo O'
_chemical_formula_weight         390.98
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9735(10)
_cell_length_b                   11.9079(4)
_cell_length_c                   8.4183(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      9.9
_cell_volume                     1400.76(14)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 Diffractometer'
_diffrn_measurement_method       'omega/2theta 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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2653
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.676
_exptl_absorpt_correction_T_max  0.6468
_exptl_absorpt_correction_T_min  0.5562
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1251
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_restrained_S_obs      0.994
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_obs          0.0334
_refine_ls_shift/esd_max         -0.028
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0573P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0837
_refine_ls_wR_factor_obs         0.0788
_reflns_number_observed          1135
_reflns_number_total             1251
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000591u_1.cif
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321664
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
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
Mo1 0.0325(2) 0.0251(2) 0.0264(2) -0.0061(3) 0.000 0.000
Cl1 0.0401(6) 0.0702(8) 0.0332(7) -0.0048(7) 0.0121(5) -0.0014(6)
Cl2 0.0778(10) 0.0430(7) 0.0639(9) -0.0114(7) -0.0077(8) 0.0320(7)
O1 0.070(5) 0.068(4) 0.064(5) -0.043(4) 0.000 0.000
C1 0.036(3) 0.022(2) 0.026(3) 0.002(2) 0.000 0.000
C2 0.027(2) 0.029(2) 0.023(2) -0.004(2) 0.001(2) -0.006(2)
C3 0.034(2) 0.025(2) 0.024(2) -0.001(2) -0.004(2) 0.005(2)
C4 0.062(4) 0.031(2) 0.038(3) 0.003(5) 0.000 0.000
C5 0.032(2) 0.060(3) 0.047(3) -0.004(3) 0.001(2) -0.013(2)
C6 0.062(3) 0.054(3) 0.041(3) 0.009(3) -0.015(3) 0.019(3)
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.0000 0.77904(3) -0.35559(3) 0.02803(14) Uani 1 d S .
Cl1 Cl -0.11650(10) 0.70003(13) -0.1769(2) 0.0478(3) Uani 1 d . .
Cl2 Cl -0.12054(12) 0.91693(11) -0.4209(3) 0.0616(4) Uani 1 d . .
O1 O 0.0000 0.8938(7) -0.1474(10) 0.067(2) Uani 1 d S .
C1 C 0.0000 0.5952(5) -0.4592(8) 0.0281(12) Uani 1 d S .
C2 C -0.0821(3) 0.6492(4) -0.5229(6) 0.0265(8) Uani 1 d . .
C3 C -0.0509(3) 0.7340(3) -0.6281(6) 0.0277(9) Uani 1 d . .
C4 C 0.0000 0.4907(5) -0.3620(14) 0.0435(15) Uani 1 d S .
H41 H 0.0000 0.4278(5) -0.4325(14) 0.080(9) Uiso 1 d SR .
H42 H 0.0564 0.4899(5) -0.2982(14) 0.080(9) Uiso 1 d R .
C5 C -0.1835(3) 0.6103(5) -0.5104(8) 0.0465(13) Uani 1 d . .
H51 H -0.1890(8) 0.5566(33) -0.4258(42) 0.080(9) Uiso 1 calc R .
H52 H -0.2025(12) 0.5760(39) -0.6086(23) 0.080(9) Uiso 1 calc R .
H53 H -0.2243(6) 0.6734(9) -0.4887(61) 0.080(9) Uiso 1 calc R .
C6 C -0.1120(5) 0.7980(4) -0.7410(8) 0.0521(15) Uani 1 d . .
H61 H -0.1121(29) 0.7610(24) -0.8423(19) 0.080(9) Uiso 1 calc R .
H62 H -0.0871(22) 0.8726(15) -0.7529(48) 0.080(9) Uiso 1 calc R .
H63 H -0.1762(10) 0.8016(37) -0.7007(31) 0.080(9) Uiso 1 calc R .
H1 H -0.0530(47) 0.9127(53) -0.1215(104) 0.063(23) Uiso 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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
O1 Mo1 C1 149.7(3) . . ?
O1 Mo1 C2 149.79(13) . . ?
C1 Mo1 C2 34.85(13) . . ?
O1 Mo1 C2 149.79(13) . 4 ?
C1 Mo1 C2 34.85(13) . 4 ?
C2 Mo1 C2 57.5(2) . 4 ?
O1 Mo1 Cl1 75.4(2) . 4 ?
C1 Mo1 Cl1 82.44(13) . 4 ?
C2 Mo1 Cl1 116.16(12) . 4 ?
C2 Mo1 Cl1 77.91(11) 4 4 ?
O1 Mo1 Cl1 75.4(2) . . ?
C1 Mo1 Cl1 82.44(13) . . ?
C2 Mo1 Cl1 77.91(11) . . ?
C2 Mo1 Cl1 116.16(12) 4 . ?
Cl1 Mo1 Cl1 85.07(8) 4 . ?
O1 Mo1 Cl2 76.2(2) . . ?
C1 Mo1 Cl2 123.17(11) . . ?
C2 Mo1 Cl2 88.32(12) . . ?
C2 Mo1 Cl2 129.90(13) 4 . ?
Cl1 Mo1 Cl2 151.54(7) 4 . ?
Cl1 Mo1 Cl2 86.35(6) . . ?
O1 Mo1 Cl2 76.2(2) . 4 ?
C1 Mo1 Cl2 123.17(11) . 4 ?
C2 Mo1 Cl2 129.90(13) . 4 ?
C2 Mo1 Cl2 88.32(12) 4 4 ?
Cl1 Mo1 Cl2 86.35(6) 4 4 ?
Cl1 Mo1 Cl2 151.54(7) . 4 ?
Cl2 Mo1 Cl2 88.42(9) . 4 ?
O1 Mo1 C3 150.4(2) . . ?
C1 Mo1 C3 56.8(2) . . ?
C2 Mo1 C3 33.83(14) . . ?
C2 Mo1 C3 56.44(14) 4 . ?
Cl1 Mo1 C3 133.83(10) 4 . ?
Cl1 Mo1 C3 107.57(11) . . ?
Cl2 Mo1 C3 74.60(11) . . ?
Cl2 Mo1 C3 97.90(12) 4 . ?
O1 Mo1 C3 150.4(2) . 4 ?
C1 Mo1 C3 56.8(2) . 4 ?
C2 Mo1 C3 56.44(14) . 4 ?
C2 Mo1 C3 33.83(14) 4 4 ?
Cl1 Mo1 C3 107.57(11) 4 4 ?
Cl1 Mo1 C3 133.83(10) . 4 ?
Cl2 Mo1 C3 97.90(12) . 4 ?
Cl2 Mo1 C3 74.60(11) 4 4 ?
C3 Mo1 C3 33.6(2) . 4 ?
Mo1 O1 H1 112.7(57) . . ?
C2 C1 C2 107.8(5) . 4 ?
C2 C1 C4 125.9(2) . . ?
C2 C1 C4 125.9(2) 4 . ?
C2 C1 Mo1 73.7(3) . . ?
C2 C1 Mo1 73.7(3) 4 . ?
C4 C1 Mo1 125.0(5) . . ?
C1 C2 C3 108.1(4) . . ?
C1 C2 C5 126.8(4) . . ?
C3 C2 C5 124.0(5) . . ?
C1 C2 Mo1 71.5(3) . . ?
C3 C2 Mo1 76.0(2) . . ?
C5 C2 Mo1 128.0(4) . . ?
C2 C3 C3 108.0(3) . 4 ?
C2 C3 C6 126.1(5) . . ?
C3 C3 C6 125.0(3) 4 . ?
C2 C3 Mo1 70.1(2) . . ?
C3 C3 Mo1 73.20(11) 4 . ?
C6 C3 Mo1 130.5(3) . . ?
C1 C4 H41 108.3(5) . . ?
C1 C4 H42 108.5(2) . . ?
H41 C4 H42 110.0 . . ?
C2 C5 H51 109.5(3) . . ?
C2 C5 H52 109.5(3) . . ?
H51 C5 H52 109.5 . . ?
C2 C5 H53 109.5(3) . . ?
H51 C5 H53 109.5 . . ?
H52 C5 H53 109.5 . . ?
C3 C6 H61 109.5(3) . . ?
C3 C6 H62 109.5(3) . . ?
H61 C6 H62 109.5 . . ?
C3 C6 H63 109.5(3) . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
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 O1 2.222(7) . ?
Mo1 C1 2.356(6) . ?
Mo1 C2 2.385(4) . ?
Mo1 C2 2.385(4) 4 ?
Mo1 Cl1 2.4080(15) 4 ?
Mo1 Cl1 2.4080(15) . ?
Mo1 Cl2 2.4156(14) . ?
Mo1 Cl2 2.4156(14) 4 ?
Mo1 C3 2.461(5) . ?
Mo1 C3 2.461(5) 4 ?
O1 H1 0.80(7) . ?
C1 C2 1.420(5) . ?
C1 C2 1.420(5) 4 ?
C1 C4 1.490(10) . ?
C2 C3 1.412(6) . ?
C2 C5 1.495(6) . ?
C3 C3 1.422(9) 4 ?
C3 C6 1.487(7) . ?
C4 H41 0.96 . ?
C4 H42 0.95 . ?
C5 H51 0.96 . ?
C5 H52 0.96 . ?
C5 H53 0.96 . ?
C6 H61 0.96 . ?
C6 H62 0.96 . ?
C6 H63 0.96 . ?
