#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/59/4315910.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_4315910
loop_
_publ_author_name
'Andrés G. Algarra'
'Manuel G. Basallote'
'M. Jesús Fernández-Trujillo'
'Marta Feliz'
'Eva Guillamón'
'Rosa Llusar'
'Ivan Sorribes'
'Cristian Vicent'
_publ_contact_author             'Rosa Llusar'
_publ_contact_author_address
;
 Departament de Química Física i Analítica, Universitat Jaume I,  
 Av. Sos Baynat s/n,  12071 Castelló de la Plana, Spain.
;
_publ_contact_author_email       llusar@exp.uji.es
_publ_contact_author_phone       '+34 964 728086'
_publ_section_title
;
 Chiral [Mo3S4H3(diphosphine)3]+ Hydrido Clusters and Study of the Effect
 of the Metal Atom on the Kinetics of the Acid-Assisted Substitution of
 the Coordinated Hydride: Mo vs W
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5935
_journal_page_last               5942
_journal_paper_doi               10.1021/ic100381u
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration syn
_chemical_formula_sum            'C42 H84 Br P6 S4 W3'
_chemical_formula_weight         1534.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.9636(10)
_cell_length_b                   14.9636(10)
_cell_length_c                   23.254(3)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.35
_cell_volume                     4509.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8163
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    6.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.758613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2241
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.646
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.043(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3780
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0301
_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)+(0.0558P)²+0.0094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                3552
_reflns_number_total             3780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100381u_si_001_3.cif
_cod_data_source_block           '[4]Br'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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_original_sg_symbol_Hall     R3
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4315910
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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_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
W1 W 0.38430(2) 0.78971(2) 0.05733(3) 0.02860(10) Uani 1 1 d . . .
S1 S 0.3333 0.6667 -0.01739(15) 0.0346(7) Uani 1 3 d S . .
S2 S 0.49858(17) 0.76258(15) 0.11403(9) 0.0351(4) Uani 1 1 d . . .
P1 P 0.44346(18) 0.95813(17) 0.10635(10) 0.0385(5) Uani 1 1 d . . .
P2 P 0.53755(18) 0.90941(17) -0.00544(10) 0.0392(5) Uani 1 1 d . . .
C1 C 0.3627(13) 1.0683(13) 0.0429(7) 0.095(5) Uani 1 1 d . . .
H1A H 0.3456 1.0205 0.0116 0.142 Uiso 1 1 calc R . .
H1B H 0.4314 1.1252 0.0376 0.142 Uiso 1 1 calc R . .
H1C H 0.3148 1.0933 0.0437 0.142 Uiso 1 1 calc R . .
C2 C 0.3568(9) 1.0136(8) 0.0999(5) 0.058(3) Uani 1 1 d . . .
H2 H 0.2856 0.9571 0.1046 0.070 Uiso 1 1 calc R . .
C3 C 0.3833(13) 1.0831(11) 0.1515(6) 0.083(4) Uani 1 1 d D . .
H3A H 0.4458 1.1482 0.1443 0.100 Uiso 1 1 calc R . .
H3B H 0.3278 1.0971 0.1595 0.100 Uiso 1 1 calc R . .
C4 C 0.398(2) 1.0310(17) 0.1999(6) 0.130(8) Uani 1 1 d D . .
H4A H 0.3311 0.9793 0.2144 0.156 Uiso 1 1 calc R . .
H4B H 0.4331 1.0808 0.2304 0.156 Uiso 1 1 calc R . .
C5 C 0.4592(9) 0.9801(8) 0.1851(4) 0.060(3) Uani 1 1 d . . .
H5 H 0.5320 1.0294 0.1928 0.072 Uiso 1 1 calc R . .
C6 C 0.4281(15) 0.8866(11) 0.2219(5) 0.089(5) Uani 1 1 d . . .
H6A H 0.4710 0.8576 0.2131 0.134 Uiso 1 1 calc R . .
H6B H 0.3573 0.8364 0.2145 0.134 Uiso 1 1 calc R . .
H6C H 0.4362 0.9062 0.2617 0.134 Uiso 1 1 calc R . .
C7 C 0.5709(8) 1.0566(7) 0.0792(5) 0.056(3) Uani 1 1 d . . .
H7A H 0.5810 1.1248 0.0865 0.067 Uiso 1 1 calc R . .
H7B H 0.6246 1.0507 0.0993 0.067 Uiso 1 1 calc R . .
C8 C 0.5783(9) 1.0423(7) 0.0151(5) 0.055(3) Uani 1 1 d . . .
H8A H 0.6492 1.0865 0.0030 0.066 Uiso 1 1 calc R . .
H8B H 0.5360 1.0643 -0.0051 0.066 Uiso 1 1 calc R . .
C9 C 0.7305(10) 0.9407(14) 0.0401(6) 0.090(5) Uani 1 1 d . . .
H9A H 0.6967 0.9098 0.0757 0.135 Uiso 1 1 calc R . .
H9B H 0.7564 1.0137 0.0415 0.135 Uiso 1 1 calc R . .
H9C H 0.7868 0.9282 0.0341 0.135 Uiso 1 1 calc R . .
C10 C 0.6574(7) 0.8960(8) -0.0068(5) 0.055(3) Uani 1 1 d . . .
H10 H 0.6333 0.8219 -0.0067 0.066 Uiso 1 1 calc R . .
C11 C 0.6979(10) 0.9356(11) -0.0685(6) 0.080(4) Uani 1 1 d . . .
H11A H 0.7338 1.0104 -0.0690 0.096 Uiso 1 1 calc R . .
H11B H 0.7463 0.9135 -0.0798 0.096 Uiso 1 1 calc R . .
C12 C 0.6127(11) 0.8953(11) -0.1085(5) 0.076(3) Uani 1 1 d . . .
H12A H 0.5814 0.8210 -0.1115 0.091 Uiso 1 1 calc R . .
H12B H 0.6367 0.9251 -0.1463 0.091 Uiso 1 1 calc R . .
C13 C 0.5339(9) 0.9235(8) -0.0859(4) 0.060(3) Uani 1 1 d . . .
H13 H 0.5609 0.9968 -0.0940 0.072 Uiso 1 1 calc R . .
C14 C 0.4247(12) 0.8622(12) -0.1144(5) 0.084(4) Uani 1 1 d . . .
H14A H 0.3799 0.8840 -0.0980 0.126 Uiso 1 1 calc R . .
H14B H 0.3965 0.7897 -0.1077 0.126 Uiso 1 1 calc R . .
H14C H 0.4307 0.8752 -0.1550 0.126 Uiso 1 1 calc R . .
Br1 Br 0.6667 0.3333 0.1520(2) 0.1562(16) Uani 1 3 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'
P P 0.1023 0.0942 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
S2 W1 S2 105.36(11) 2_665 . ?
S2 W1 S1 105.40(6) 2_665 . ?
S2 W1 S1 104.90(6) . . ?
S2 W1 P1 83.51(8) 2_665 . ?
S2 W1 P1 89.82(8) . . ?
S1 W1 P1 159.66(7) . . ?
S2 W1 P2 158.02(7) 2_665 . ?
S2 W1 P2 88.05(8) . . ?
S1 W1 P2 87.30(7) . . ?
P1 W1 P2 79.12(7) . . ?
S2 W1 W1 53.92(5) 2_665 2_665 ?
S2 W1 W1 101.50(5) . 2_665 ?
S1 W1 W1 54.05(5) . 2_665 ?
P1 W1 W1 137.42(5) . 2_665 ?
P2 W1 W1 141.34(5) . 2_665 ?
S2 W1 W1 101.90(5) 2_665 3_565 ?
S2 W1 W1 53.41(5) . 3_565 ?
S1 W1 W1 54.05(5) . 3_565 ?
P1 W1 W1 143.11(6) . 3_565 ?
P2 W1 W1 100.08(5) . 3_565 ?
W1 W1 W1 60.0 2_665 3_565 ?
W1 S1 W1 71.90(9) . 2_665 ?
W1 S1 W1 71.90(9) . 3_565 ?
W1 S1 W1 71.90(9) 2_665 3_565 ?
W1 S2 W1 72.67(6) 3_565 . ?
C7 P1 C5 102.0(5) . . ?
C7 P1 C2 106.8(5) . . ?
C5 P1 C2 93.2(5) . . ?
C7 P1 W1 110.8(3) . . ?
C5 P1 W1 125.5(4) . . ?
C2 P1 W1 116.1(4) . . ?
C8 P2 C13 98.7(5) . . ?
C8 P2 C10 107.4(5) . . ?
C13 P2 C10 94.4(5) . . ?
C8 P2 W1 108.0(3) . . ?
C13 P2 W1 125.5(4) . . ?
C10 P2 W1 120.0(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 113.3(10) . . ?
C3 C2 P1 104.0(8) . . ?
C1 C2 P1 116.0(8) . . ?
C3 C2 H2 107.7 . . ?
C1 C2 H2 107.7 . . ?
P1 C2 H2 107.7 . . ?
C4 C3 C2 107.8(11) . . ?
C4 C3 H3A 110.1 . . ?
C2 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
C2 C3 H3B 110.1 . . ?
H3A C3 H3B 108.5 . . ?
C3 C4 C5 113.1(11) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C4 111.1(13) . . ?
C6 C5 P1 116.5(8) . . ?
C4 C5 P1 105.2(9) . . ?
C6 C5 H5 107.9 . . ?
C4 C5 H5 107.9 . . ?
P1 C5 H5 107.9 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P1 110.1(7) . . ?
C8 C7 H7A 109.6 . . ?
P1 C7 H7A 109.7 . . ?
C8 C7 H7B 109.6 . . ?
P1 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 P2 113.7(6) . . ?
C7 C8 H8A 108.8 . . ?
P2 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
P2 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C9 C10 C11 117.2(10) . . ?
C9 C10 P2 118.2(9) . . ?
C11 C10 P2 100.7(8) . . ?
C9 C10 H10 106.6 . . ?
C11 C10 H10 106.6 . . ?
P2 C10 H10 106.6 . . ?
C12 C11 C10 109.9(9) . . ?
C12 C11 H11A 109.7 . . ?
C10 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
C10 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C11 C12 C13 107.8(10) . . ?
C11 C12 H12A 110.1 . . ?
C13 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
C13 C12 H12B 110.1 . . ?
H12A C12 H12B 108.5 . . ?
C12 C13 C14 114.5(11) . . ?
C12 C13 P2 103.9(8) . . ?
C14 C13 P2 115.8(8) . . ?
C12 C13 H13 107.4 . . ?
C14 C13 H13 107.4 . . ?
P2 C13 H13 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
W1 S2 2.334(2) 2_665 ?
W1 S2 2.350(2) . ?
W1 S1 2.364(3) . ?
W1 P1 2.491(2) . ?
W1 P2 2.548(2) . ?
W1 W1 2.7753(5) 2_665 ?
W1 W1 2.7753(5) 3_565 ?
S1 W1 2.364(3) 2_665 ?
S1 W1 2.364(3) 3_565 ?
S2 W1 2.334(2) 3_565 ?
P1 C7 1.842(10) . ?
P1 C5 1.855(10) . ?
P1 C2 1.863(10) . ?
P2 C8 1.827(9) . ?
P2 C13 1.886(11) . ?
P2 C10 1.902(10) . ?
C1 C2 1.537(19) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.506(17) . ?
C2 H2 0.9800 . ?
C3 C4 1.447(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.495(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.501(17) . ?
C5 H5 0.9800 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.518(15) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.450(17) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.554(16) . ?
C10 H10 0.9800 . ?
C11 C12 1.44(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.530(16) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.566(18) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
