#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:43:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179259 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/79/4317941.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_4317941
loop_
_publ_author_name
'Raquel Garcia'
'Ângela Domingos'
'António Paulo'
'Isabel Santos'
'Roger Alberto'
_publ_section_title
;
 Reactivity of [Re{κ3-H(μ-H)B(timMe)2}(CO)3] (timMe=
 2-Mercapto-1-methylimidazolyl) toward Neutral Substrates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2422
_journal_page_last               2428
_journal_paper_doi               10.1021/ic011171n
_journal_volume                  41
_journal_year                    2002
_chemical_formula_structural     '[Re{k2-H2B(MeC3H2N2S)2}(CO)3(PPh3)]'
_chemical_formula_sum            'C29 H27 B N4 O3 P Re S2'
_chemical_formula_weight         771.65
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   10.3595(4)
_cell_length_b                   18.0988(12)
_cell_length_c                   33.845(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      10.4
_cell_volume                     6345.8(6)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius'1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MolEN(Fair,1990)
_computing_molecular_graphics    ORTEP-3(Farrugia,1997)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4-Enraf-Nonius
_diffrn_measurement_method       ω/2\qscans
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5559
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.048
_exptl_absorpt_correction_T_max  0.9994
_exptl_absorpt_correction_T_min  0.9515
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.187
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      2.016
_refine_ls_restrained_S_obs      1.186
_refine_ls_R_factor_all          0.1705
_refine_ls_R_factor_obs          0.0591
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0399P)²+29.3976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2627
_refine_ls_wR_factor_obs         0.1020
_reflns_number_observed          2525
_reflns_number_total             5559
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011171n_2.cif
_cod_data_source_block           refosfina
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+29.3976P] 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^)+(0.0399P)^2^+29.3976P] 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               4317941
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'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re 0.00208(7) 0.08275(3) 0.127354(14) 0.0382(2) Uani 1 d . .
S1 S 0.0061(5) -0.0573(2) 0.12083(10) 0.0452(8) Uani 1 d . .
S2 S 0.1672(4) 0.0697(2) 0.18168(12) 0.0428(10) Uani 1 d . .
P1 P 0.1972(4) 0.0914(2) 0.08421(11) 0.0378(9) Uani 1 d . .
O1 O -0.0273(14) 0.2508(7) 0.1327(5) 0.121(6) Uani 1 d . .
O2 O -0.1993(12) 0.0847(10) 0.0618(4) 0.113(6) Uani 1 d . .
O3 O -0.2175(10) 0.0764(7) 0.1888(3) 0.070(4) Uani 1 d . .
N1 N -0.0909(12) -0.0991(6) 0.1932(4) 0.044(3) Uani 1 d . .
N2 N -0.2328(12) -0.1007(7) 0.1460(4) 0.058(4) Uani 1 d . .
N3 N 0.0296(10) -0.0094(6) 0.2372(3) 0.041(3) Uani 1 d . .
N4 N 0.0463(13) 0.1071(6) 0.2505(4) 0.057(4) Uani 1 d . .
C1 C -0.0124(21) 0.1868(9) 0.1314(6) 0.075(5) Uani 1 d . .
C2 C -0.1167(17) 0.0835(11) 0.0852(5) 0.069(5) Uani 1 d . .
C3 C -0.1352(15) 0.0776(10) 0.1663(4) 0.048(4) Uani 1 d . .
C4 C -0.1091(14) -0.0850(8) 0.1546(4) 0.045(4) Uani 1 d . .
C5 C -0.2040(18) -0.1230(8) 0.2092(5) 0.061(5) Uani 1 d . .
H5 H -0.2169(18) -0.1378(8) 0.2353(5) 0.073 Uiso 1 calc R .
C6 C -0.2936(16) -0.1214(9) 0.1804(5) 0.063(5) Uani 1 d . .
H6 H -0.3808(16) -0.1324(9) 0.1832(5) 0.075 Uiso 1 calc R .
C7 C -0.2925(17) -0.0905(11) 0.1077(5) 0.086(6) Uani 1 d . .
H7A H -0.3812(17) -0.1056(11) 0.1090(5) 0.129 Uiso 1 calc R .
H7B H -0.2479(17) -0.1198(11) 0.0884(5) 0.129 Uiso 1 calc R .
H7C H -0.2880(17) -0.0394(11) 0.1004(5) 0.129 Uiso 1 calc R .
C8 C 0.0784(13) 0.0532(8) 0.2240(4) 0.037(3) Uani 1 d . .
C9 C -0.0346(14) 0.0071(10) 0.2718(4) 0.053(5) Uani 1 d . .
H9 H -0.0793(14) -0.0272(10) 0.2870(4) 0.063 Uiso 1 calc R .
C10 C -0.0244(18) 0.0780(10) 0.2806(4) 0.071(6) Uani 1 d . .
H10 H -0.0580(18) 0.1025(10) 0.3024(4) 0.085 Uiso 1 calc R .
C11 C 0.0844(21) 0.1850(8) 0.2463(6) 0.092(7) Uani 1 d . .
H11A H 0.1338(21) 0.1911(8) 0.2225(6) 0.137 Uiso 1 calc R .
H11B H 0.1358(21) 0.1993(8) 0.2686(6) 0.137 Uiso 1 calc R .
H11C H 0.0086(21) 0.2154(8) 0.2451(6) 0.137 Uiso 1 calc R .
C100 C 0.3306(13) 0.1423(7) 0.1055(4) 0.031(3) Uani 1 d . .
C101 C 0.3095(16) 0.2071(8) 0.1267(5) 0.062(5) Uani 1 d . .
H101 H 0.2256(16) 0.2238(8) 0.1307(5) 0.074 Uiso 1 calc R .
C102 C 0.4108(18) 0.2464(9) 0.1416(5) 0.068(6) Uani 1 d . .
H102 H 0.3940(18) 0.2913(9) 0.1539(5) 0.082 Uiso 1 calc R .
C103 C 0.5363(15) 0.2226(9) 0.1393(5) 0.057(5) Uani 1 d . .
H103 H 0.6037(15) 0.2493(9) 0.1505(5) 0.068 Uiso 1 calc R .
C104 C 0.5573(15) 0.1578(9) 0.1198(5) 0.052(4) Uani 1 d . .
H104 H 0.6414(15) 0.1403(9) 0.1173(5) 0.062 Uiso 1 calc R .
C105 C 0.4582(14) 0.1177(8) 0.1038(5) 0.055(5) Uani 1 d . .
H105 H 0.4764(14) 0.0729(8) 0.0915(5) 0.066 Uiso 1 calc R .
C110 C 0.1684(17) 0.1382(9) 0.0368(4) 0.051(4) Uani 1 d . .
C111 C 0.0688(17) 0.1147(10) 0.0139(4) 0.067(5) Uani 1 d . .
H111 H 0.0137(17) 0.0772(10) 0.0223(4) 0.080 Uiso 1 calc R .
C112 C 0.0525(24) 0.1496(15) -0.0231(6) 0.107(9) Uani 1 d . .
H112 H -0.0097(24) 0.1321(15) -0.0406(6) 0.129 Uiso 1 calc R .
C113 C 0.1263(35) 0.2082(15) -0.0334(6) 0.126(14) Uani 1 d . .
H113 H 0.1087(35) 0.2339(15) -0.0565(6) 0.152 Uiso 1 calc R .
C114 C 0.2235(33) 0.2289(13) -0.0106(6) 0.126(12) Uani 1 d . .
H114 H 0.2762(33) 0.2675(13) -0.0189(6) 0.152 Uiso 1 calc R .
C115 C 0.2483(22) 0.1957(9) 0.0242(5) 0.073(6) Uani 1 d . .
H115 H 0.3177(22) 0.2108(9) 0.0397(5) 0.088 Uiso 1 calc R .
C120 C 0.2723(12) 0.0036(7) 0.0702(5) 0.043(4) Uani 1 d . .
C121 C 0.3025(13) -0.0454(8) 0.0999(5) 0.046(4) Uani 1 d . .
H121 H 0.2819(13) -0.0345(8) 0.1260(5) 0.056 Uiso 1 calc R .
C122 C 0.3638(14) -0.1110(9) 0.0905(6) 0.063(5) Uani 1 d . .
H122 H 0.3820(14) -0.1450(9) 0.1103(6) 0.075 Uiso 1 calc R .
C123 C 0.3975(19) -0.1262(11) 0.0529(7) 0.089(7) Uani 1 d . .
H123 H 0.4405(19) -0.1701(11) 0.0472(7) 0.106 Uiso 1 calc R .
C124 C 0.3689(21) -0.0774(12) 0.0228(6) 0.093(7) Uani 1 d . .
H124 H 0.3900(21) -0.0888(12) -0.0032(6) 0.111 Uiso 1 calc R .
C125 C 0.3100(15) -0.0128(9) 0.0315(5) 0.065(5) Uani 1 d . .
H125 H 0.2942(15) 0.0212(9) 0.0115(5) 0.078 Uiso 1 calc R .
B1 B 0.0364(14) -0.0861(10) 0.2183(5) 0.046(4) Uani 1 d D .
H1A H 0.0440(14) -0.1252(10) 0.2395(5) 0.055 Uiso 1 calc RD .
H1B H 0.1147(14) -0.0896(10) 0.2006(5) 0.055 Uiso 1 calc RD .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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
C2 Re1 C1 89.8(9) . . ?
C2 Re1 C3 92.0(6) . . ?
C1 Re1 C3 86.6(8) . . ?
C2 Re1 P1 94.9(5) . . ?
C1 Re1 P1 92.5(6) . . ?
C3 Re1 P1 173.0(4) . . ?
C2 Re1 S2 174.6(6) . . ?
C1 Re1 S2 95.4(6) . . ?
C3 Re1 S2 89.9(4) . . ?
P1 Re1 S2 83.29(13) . . ?
C2 Re1 S1 87.2(6) . . ?
C1 Re1 S1 176.3(6) . . ?
C3 Re1 S1 91.3(5) . . ?
P1 Re1 S1 89.93(13) . . ?
S2 Re1 S1 87.65(13) . . ?
C4 S1 Re1 102.8(5) . . ?
C8 S2 Re1 105.0(5) . . ?
C100 P1 C120 102.7(6) . . ?
C100 P1 C110 103.7(7) . . ?
C120 P1 C110 104.0(7) . . ?
C100 P1 Re1 114.6(4) . . ?
C120 P1 Re1 116.1(5) . . ?
C110 P1 Re1 114.1(5) . . ?
C4 N1 C5 109.1(14) . . ?
C4 N1 B1 127.5(12) . . ?
C5 N1 B1 123.3(13) . . ?
C4 N2 C6 108.0(14) . . ?
C4 N2 C7 125.1(14) . . ?
C6 N2 C7 126.6(14) . . ?
C8 N3 C9 106.6(12) . . ?
C8 N3 B1 128.3(12) . . ?
C9 N3 B1 125.0(13) . . ?
C10 N4 C8 110.2(13) . . ?
C10 N4 C11 126.0(14) . . ?
C8 N4 C11 123.8(14) . . ?
O1 C1 Re1 176.3(21) . . ?
O2 C2 Re1 173.6(15) . . ?
O3 C3 Re1 178.1(16) . . ?
N1 C4 N2 107.7(14) . . ?
N1 C4 S1 127.0(11) . . ?
N2 C4 S1 125.1(12) . . ?
C6 C5 N1 107.3(14) . . ?
C5 C6 N2 107.7(14) . . ?
N3 C8 N4 107.3(12) . . ?
N3 C8 S2 129.3(11) . . ?
N4 C8 S2 123.3(11) . . ?
C10 C9 N3 111.2(14) . . ?
C9 C10 N4 104.6(14) . . ?
C101 C100 C105 116.0(13) . . ?
C101 C100 P1 120.9(11) . . ?
C105 C100 P1 123.0(10) . . ?
C102 C101 C100 120.6(15) . . ?
C101 C102 C103 123.0(16) . . ?
C104 C103 C102 116.7(15) . . ?
C103 C104 C105 121.9(14) . . ?
C104 C105 C100 121.6(13) . . ?
C111 C110 C115 120.8(15) . . ?
C111 C110 P1 118.4(14) . . ?
C115 C110 P1 120.8(13) . . ?
C110 C111 C112 117.1(20) . . ?
C113 C112 C111 120.7(23) . . ?
C114 C113 C112 120.2(24) . . ?
C113 C114 C115 121.9(28) . . ?
C114 C115 C110 119.0(22) . . ?
C121 C120 C125 118.9(14) . . ?
C121 C120 P1 117.9(12) . . ?
C125 C120 P1 123.0(12) . . ?
C120 C121 C122 119.3(15) . . ?
C123 C122 C121 120.8(18) . . ?
C122 C123 C124 120.6(18) . . ?
C125 C124 C123 119.3(18) . . ?
C124 C125 C120 121.0(18) . . ?
N3 B1 N1 108.6(11) . . ?
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
Re1 C2 1.88(2) . ?
Re1 C1 1.89(2) . ?
Re1 C3 1.94(2) . ?
Re1 P1 2.498(4) . ?
Re1 S2 2.523(4) . ?
Re1 S1 2.544(3) . ?
S1 C4 1.73(2) . ?
S2 C8 1.727(14) . ?
P1 C100 1.810(13) . ?
P1 C120 1.832(13) . ?
P1 C110 1.840(14) . ?
O1 C1 1.17(2) . ?
O2 C2 1.17(2) . ?
O3 C3 1.14(2) . ?
N1 C4 1.34(2) . ?
N1 C5 1.36(2) . ?
N1 B1 1.59(2) . ?
N2 C4 1.34(2) . ?
N2 C6 1.38(2) . ?
N2 C7 1.45(2) . ?
N3 C8 1.32(2) . ?
N3 C9 1.38(2) . ?
N3 B1 1.53(2) . ?
N4 C10 1.36(2) . ?
N4 C8 1.37(2) . ?
N4 C11 1.47(2) . ?
C5 C6 1.35(2) . ?
C9 C10 1.32(2) . ?
C100 C101 1.39(2) . ?
C100 C105 1.40(2) . ?
C101 C102 1.36(2) . ?
C102 C103 1.37(2) . ?
C103 C104 1.36(2) . ?
C104 C105 1.37(2) . ?
C110 C111 1.36(2) . ?
C110 C115 1.40(2) . ?
C111 C112 1.41(2) . ?
C112 C113 1.35(3) . ?
C113 C114 1.32(4) . ?
C114 C115 1.35(2) . ?
C120 C121 1.37(2) . ?
C120 C125 1.40(2) . ?
C121 C122 1.38(2) . ?
C122 C123 1.35(2) . ?
C123 C124 1.38(3) . ?
C124 C125 1.35(2) . ?
