#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/92/2009284.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009284
loop_
_publ_author_name
'Wei, Qiang'
'Zhuang, Botao'
'Chen, Jiutong'
_publ_section_title
;
 A long-chain alkyl-tethered Mo₂S₂ core,
 [Bu₄N]₂[Mo₂(CO)₈(n-C₆H₁₃ S)₂]
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2047
_journal_page_last               2049
_journal_paper_doi               10.1107/S0108270199011191
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '(C16 H36 N)2 [Mo2 (C6 H13 S)2 (CO)8 ]'
_chemical_formula_moiety         '2C16 H36 N + , C20 H26 Mo2 O8 S2 2-'
_chemical_formula_sum            'C52 H98 Mo2 N2 O8 S2'
_chemical_formula_weight         1135.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.0330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4702(2)
_cell_length_b                   15.8641(3)
_cell_length_c                   16.9102(3)
_cell_measurement_reflns_used    7613
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.73
_cell_volume                     3162.43(10)
_computing_cell_refinement       'SMART and  SAINT (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'XPREP in SHELXTL'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'ω 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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11821
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0544P)²+0.7794P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1144
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                4240
_reflns_number_total             5415
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ja1002.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3162.43(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2009284
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Mo 0.62300(2) 0.54334(2) 0.09911(2) 0.05503(13) Uani d . 1 . Mo
S 0.49356(8) 0.41134(6) 0.05233(5) 0.0582(2) Uani d . 1 . S
O1 0.4503(3) 0.6208(3) 0.1819(3) 0.1245(13) Uani d . 1 . O
O2 0.7659(3) 0.7074(2) 0.1348(2) 0.1083(11) Uani d . 1 . O
O3 0.7624(3) 0.4913(3) 0.2812(2) 0.1126(12) Uani d . 1 . O
O4 0.8167(3) 0.4582(2) 0.0443(2) 0.0982(10) Uani d . 1 . O
C1 0.5077(4) 0.5936(3) 0.1485(3) 0.0748(11) Uani d . 1 . C
C2 0.7102(3) 0.6459(3) 0.1213(2) 0.0726(11) Uani d . 1 . C
C3 0.7095(3) 0.5084(3) 0.2127(3) 0.0738(11) Uani d . 1 . C
C4 0.7440(3) 0.4889(3) 0.0611(2) 0.0645(9) Uani d . 1 . C
C11 0.5771(4) 0.3184(2) 0.0464(2) 0.0739(11) Uani d . 1 . C
H11A 0.5265(4) 0.2748(2) 0.0149(2) 0.089 Uiso calc R 1 . H
H11B 0.6287(4) 0.3329(2) 0.0162(2) 0.089 Uiso calc R 1 . H
C12 0.6450(5) 0.2838(3) 0.1314(3) 0.109(2) Uani d D 1 . C
H12A 0.7048(5) 0.3235(3) 0.1586(3) 0.131 Uiso calc R 1 . H
H12B 0.5957(5) 0.2796(3) 0.1653(3) 0.131 Uiso calc R 1 . H
C13 0.6978(6) 0.1987(4) 0.1292(4) 0.152(3) Uani d D 1 . C
H13A 0.7269(6) 0.1776(4) 0.1861(4) 0.182 Uiso calc R 1 . H
H13B 0.6384(6) 0.1605(4) 0.0979(4) 0.182 Uiso calc R 1 . H
C14 0.7883(6) 0.1952(5) 0.0936(5) 0.163(3) Uani d D 1 . C
H14A 0.8459(6) 0.2361(5) 0.1215(5) 0.196 Uiso calc R 1 . H
H14B 0.7585(6) 0.2104(5) 0.0349(5) 0.196 Uiso calc R 1 . H
C15 0.8418(9) 0.1093(5) 0.1014(7) 0.204(4) Uani d D 1 . C
H15A 0.8849(9) 0.0991(5) 0.1596(7) 0.244 Uiso calc R 1 . H
H15B 0.7823(9) 0.0672(5) 0.0843(7) 0.244 Uiso calc R 1 . H
C16 0.9160(9) 0.0990(6) 0.0519(8) 0.236(5) Uani d D 1 . C
H16A 0.9473(9) 0.0431(6) 0.0597(8) 0.354 Uiso calc R 1 . H
H16B 0.9764(9) 0.1394(6) 0.0693(8) 0.354 Uiso calc R 1 . H
H16C 0.8737(9) 0.1075(6) -0.0061(8) 0.354 Uiso calc R 1 . H
N 1.2030(2) 0.3226(2) 0.1407(2) 0.0625(8) Uani d . 1 . N
C31 1.1447(3) 0.3623(3) 0.0554(2) 0.0707(10) Uani d . 1 . C
H31A 1.1955(3) 0.3581(3) 0.0228(2) 0.085 Uiso calc R 1 . H
H31B 1.1336(3) 0.4218(3) 0.0637(2) 0.085 Uiso calc R 1 . H
C32 1.0308(4) 0.3246(3) 0.0044(3) 0.0843(12) Uani d . 1 . C
H32A 1.0414(4) 0.2663(3) -0.0089(3) 0.101 Uiso calc R 1 . H
H32B 0.9799(4) 0.3254(3) 0.0373(3) 0.101 Uiso calc R 1 . H
C33 0.9784(4) 0.3734(3) -0.0755(3) 0.0989(15) Uani d . 1 . C
H33A 0.9748(4) 0.4325(3) -0.0620(3) 0.119 Uiso calc R 1 . H
H33B 1.0267(4) 0.3684(3) -0.1101(3) 0.119 Uiso calc R 1 . H
C34 0.8614(5) 0.3433(4) -0.1243(4) 0.134(2) Uani d . 1 . C
H34A 0.8322(5) 0.3764(4) -0.1743(4) 0.201 Uiso calc R 1 . H
H34B 0.8127(5) 0.3492(4) -0.0909(4) 0.201 Uiso calc R 1 . H
H34C 0.8646(5) 0.2851(4) -0.1390(4) 0.201 Uiso calc R 1 . H
C41 1.1278(3) 0.3269(2) 0.1957(2) 0.0661(10) Uani d . 1 . C
H41A 1.0596(3) 0.2945(2) 0.1690(2) 0.079 Uiso calc R 1 . H
H41B 1.1673(3) 0.2996(2) 0.2485(2) 0.079 Uiso calc R 1 . H
C42 1.0929(4) 0.4139(3) 0.2141(3) 0.0864(12) Uani d . 1 . C
H42A 1.1586(4) 0.4431(3) 0.2509(3) 0.104 Uiso calc R 1 . H
H42B 1.0657(4) 0.4456(3) 0.1623(3) 0.104 Uiso calc R 1 . H
C43 1.0014(5) 0.4115(4) 0.2544(3) 0.103(2) Uani d . 1 . C
H43A 0.9789(5) 0.4690(4) 0.2604(3) 0.124 Uiso calc R 1 . H
H43B 0.9359(5) 0.3830(4) 0.2164(3) 0.124 Uiso calc R 1 . H
C44 1.0300(6) 0.3708(4) 0.3351(4) 0.147(3) Uani d . 1 . C
H44A 0.9659(6) 0.3729(4) 0.3547(4) 0.220 Uiso calc R 1 . H
H44B 1.0931(6) 0.3993(4) 0.3742(4) 0.220 Uiso calc R 1 . H
H44C 1.0499(6) 0.3130(4) 0.3301(4) 0.220 Uiso calc R 1 . H
C51 1.2283(3) 0.2299(2) 0.1317(2) 0.0677(10) Uani d . 1 . C
H51A 1.2666(3) 0.2073(2) 0.1870(2) 0.081 Uiso calc R 1 . H
H51B 1.1567(3) 0.2002(2) 0.1093(2) 0.081 Uiso calc R 1 . H
C52 1.2997(4) 0.2105(3) 0.0767(3) 0.0864(13) Uani d . 1 . C
H52A 1.2624(4) 0.2324(3) 0.0209(3) 0.104 Uiso calc R 1 . H
H52B 1.3727(4) 0.2382(3) 0.0992(3) 0.104 Uiso calc R 1 . H
C53 1.3172(5) 0.1174(3) 0.0720(4) 0.108(2) Uani d . 1 . C
H53A 1.2439(5) 0.0897(3) 0.0539(4) 0.130 Uiso calc R 1 . H
H53B 1.3591(5) 0.0966(3) 0.1274(4) 0.130 Uiso calc R 1 . H
C54 1.3809(5) 0.0942(4) 0.0127(4) 0.129(2) Uani d . 1 . C
H54A 1.3896(5) 0.0341(4) 0.0122(4) 0.194 Uiso calc R 1 . H
H54B 1.4543(5) 0.1204(4) 0.0309(4) 0.194 Uiso calc R 1 . H
H54C 1.3391(5) 0.1134(4) -0.0426(4) 0.194 Uiso calc R 1 . H
C61 1.3118(3) 0.3723(3) 0.1795(2) 0.0685(10) Uani d . 1 . C
H61A 1.3524(3) 0.3743(3) 0.1394(2) 0.082 Uiso calc R 1 . H
H61B 1.2915(3) 0.4298(3) 0.1881(2) 0.082 Uiso calc R 1 . H
C62 1.3915(4) 0.3398(3) 0.2609(3) 0.0831(12) Uani d . 1 . C
H62A 1.4183(4) 0.2842(3) 0.2525(3) 0.100 Uiso calc R 1 . H
H62B 1.3516(4) 0.3349(3) 0.3013(3) 0.100 Uiso calc R 1 . H
C63 1.4919(4) 0.3987(4) 0.2946(3) 0.0997(15) Uani d . 1 . C
H63A 1.5216(4) 0.4121(4) 0.2497(3) 0.120 Uiso calc R 1 . H
H63B 1.4656(4) 0.4508(4) 0.3119(3) 0.120 Uiso calc R 1 . H
C64 1.5855(5) 0.3641(4) 0.3663(4) 0.133(2) Uani d . 1 . C
H64A 1.6456(5) 0.4047(4) 0.3841(4) 0.200 Uiso calc R 1 . H
H64B 1.6136(5) 0.3132(4) 0.3494(4) 0.200 Uiso calc R 1 . H
H64C 1.5575(5) 0.3520(4) 0.4117(4) 0.200 Uiso calc R 1 . H
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 Mo C3 . . 87.3(2) yes
C2 Mo C4 . . 89.4(2) yes
C3 Mo C4 . . 87.8(2) yes
C2 Mo C1 . . 91.0(2) yes
C3 Mo C1 . . 86.9(2) yes
C4 Mo C1 . . 174.6(2) yes
C2 Mo S . 3_665 93.28(12) yes
C3 Mo S . 3_665 179.45(13) yes
C4 Mo S . 3_665 92.33(11) yes
C1 Mo S . 3_665 93.00(12) yes
C2 Mo S . . 173.55(12) yes
C3 Mo S . . 99.19(14) yes
C4 Mo S . . 90.76(11) yes
C1 Mo S . . 89.37(12) yes
S Mo S 3_665 . 80.28(3) yes
C2 Mo Mo . 3_665 133.46(12) yes
C3 Mo Mo . 3_665 139.28(14) yes
C4 Mo Mo . 3_665 92.02(11) yes
C1 Mo Mo . 3_665 91.55(12) yes
S Mo Mo 3_665 3_665 40.18(2) yes
S Mo Mo . 3_665 40.10(2) yes
C11 S Mo . 3_665 108.35(13) yes
C11 S Mo . . 110.94(14) yes
Mo S Mo 3_665 . 99.72(3) yes
O1 C1 Mo . . 174.5(4) no
O2 C2 Mo . . 178.2(4) no
O3 C3 Mo . . 176.9(4) no
O4 C4 Mo . . 176.0(3) no
C12 C11 S . . 113.2(3) no
C13 C12 C11 . . 114.6(4) no
C14 C13 C12 . . 116.9(7) no
C13 C14 C15 . . 112.6(8) no
C16 C15 C14 . . 113.7(9) no
C61 N C41 . . 110.8(3) no
C61 N C51 . . 111.0(3) no
C41 N C51 . . 107.1(3) no
C61 N C31 . . 106.1(3) no
C41 N C31 . . 111.1(3) no
C51 N C31 . . 110.8(3) no
N C31 C32 . . 116.3(3) no
C33 C32 C31 . . 110.9(4) no
C34 C33 C32 . . 112.9(5) no
C42 C41 N . . 116.3(3) no
C43 C42 C41 . . 112.4(4) no
C44 C43 C42 . . 116.6(5) no
C52 C51 N . . 116.1(3) no
C53 C52 C51 . . 111.0(4) no
C52 C53 C54 . . 113.1(4) no
C62 C61 N . . 116.6(3) no
C61 C62 C63 . . 110.5(4) no
C64 C63 C62 . . 114.2(5) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo C2 . 1.925(4) yes
Mo C3 . 1.951(4) yes
Mo C4 . 2.017(4) yes
Mo C1 . 2.046(4) yes
Mo S 3_665 2.6000(9) yes
Mo S . 2.6045(9) yes
Mo Mo 3_665 3.9788(6) yes
S C11 . 1.827(4) no
S Mo 3_665 2.6000(9) no
O1 C1 . 1.131(5) no
O2 C2 . 1.175(5) no
O3 C3 . 1.163(5) no
O4 C4 . 1.144(5) no
C11 C12 . 1.513(6) no
C12 C13 . 1.507(6) no
C13 C14 . 1.443(7) no
C14 C15 . 1.504(7) no
C15 C16 . 1.445(8) no
N C61 . 1.521(5) no
N C41 . 1.522(4) no
N C51 . 1.523(5) no
N C31 . 1.523(4) no
C31 C32 . 1.524(6) no
C32 C33 . 1.508(6) no
C33 C34 . 1.500(7) no
C41 C42 . 1.510(6) no
C42 C43 . 1.508(6) no
C43 C44 . 1.447(7) no
C51 C52 . 1.513(5) no
C52 C53 . 1.499(6) no
C53 C54 . 1.513(7) no
C61 C62 . 1.503(5) no
C62 C63 . 1.516(6) no
C63 C64 . 1.488(7) no
