#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:03:17 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179823 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/19/7011994.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_7011994
loop_
_publ_author_name
'Raquel Garcia'
'Yong-Heng Xing'
'António Paulo'
'Ângela Domingos'
'Isabel Santos'
_publ_section_title
;
 Rhenium(I) tricarbonyl complexes with mercaptoimidazolylborate ligands
 bearing piperazine fragments
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4236
_journal_page_last               4241
_journal_paper_doi               10.1039/b206603n
_journal_year                    2002
_chemical_formula_structural     '[Re{k3-Ph(u-H)B(timMe,pip)2}(CO)3].C4H8O.H2O'
_chemical_formula_sum            'C39 H50 B N8 O9 Re S2'
_chemical_formula_weight         1036.00
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   18.068(3)
_cell_length_b                   27.733(4)
_cell_length_c                   9.1500(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      8.2
_cell_volume                     4584.9(11)
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4585
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.5841
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.935
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1600
_refine_ls_R_factor_obs          0.0700
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0769P)²+26.8383P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3496
_refine_ls_wR_factor_obs         0.1487
_reflns_number_observed          2338
_reflns_number_total             4125
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b206603n.txt
_cod_data_source_block           retiml2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+26.8383P] 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^)+(0.0769P)^2^+26.8383P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7011994
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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 0.17009(4) 0.2500 0.06404(9) 0.0527(3) Uani 1 d S .
S1 S 0.1856(2) 0.31122(13) 0.2590(4) 0.0611(10) Uani 1 d . .
O2 O 0.1565(8) 0.3286(5) -0.1654(15) 0.119(5) Uani 1 d . .
N11 N 0.3308(5) 0.2956(3) 0.1908(10) 0.043(2) Uani 1 d . .
N12 N 0.3116(5) 0.3552(3) 0.3455(10) 0.045(2) Uani 1 d . .
C2 C 0.1610(7) 0.2988(6) -0.0804(18) 0.071(4) Uani 1 d . .
C11 C 0.2789(6) 0.3198(4) 0.2667(13) 0.042(3) Uani 1 d . .
O4 O 0.6579(5) 0.4615(3) -0.0817(9) 0.066(2) Uani 1 d . .
N2 N 0.5960(5) 0.4678(3) 0.1839(10) 0.041(2) Uani 1 d . .
C13 C 0.3982(6) 0.3179(4) 0.2204(12) 0.040(3) Uani 1 d . .
H13 H 0.4436(6) 0.3088(4) 0.1812(12) 0.048 Uiso 1 calc R .
N1 N 0.5031(5) 0.3982(4) 0.3188(10) 0.051(3) Uani 1 d . .
C5 C 0.5810(7) 0.4707(5) 0.3417(13) 0.059(4) Uani 1 d . .
H5A H 0.5391(7) 0.4918(5) 0.3594(13) 0.070 Uiso 1 calc R .
H5B H 0.6237(7) 0.4839(5) 0.3921(13) 0.070 Uiso 1 calc R .
O3 O 0.4314(5) 0.3941(4) 0.5195(11) 0.081(3) Uani 1 d . .
C3 C 0.4418(7) 0.3849(5) 0.3929(14) 0.053(3) Uani 1 d . .
C12 C 0.3879(6) 0.3537(4) 0.3122(13) 0.042(3) Uani 1 d . .
C9 C 0.6617(6) 0.5055(4) -0.0148(14) 0.045(3) Uani 1 d . .
B1 B 0.3236(12) 0.2500 0.0960(23) 0.055(5) Uani 1 d SD .
H1A H 0.2739(12) 0.2500 0.0452(23) 0.067 Uiso 1 calc SRD .
H1B H 0.3635(12) 0.2500 0.0186(23) 0.067 Uiso 1 calc SRD .
C14 C 0.2715(7) 0.3892(4) 0.4340(15) 0.063(4) Uani 1 d . .
H14A H 0.3057(7) 0.4110(4) 0.4798(15) 0.095 Uiso 1 calc R .
H14B H 0.2441(7) 0.3722(4) 0.5077(15) 0.095 Uiso 1 calc R .
H14C H 0.2379(7) 0.4071(4) 0.3735(15) 0.095 Uiso 1 calc R .
C16 C 0.6651(9) 0.5922(5) 0.1258(19) 0.082(5) Uani 1 d . .
H16 H 0.6651(9) 0.6217(5) 0.1743(19) 0.098 Uiso 1 calc R .
C10 C 0.6972(7) 0.5443(6) -0.0787(15) 0.066(4) Uani 1 d . .
H10 H 0.7191(7) 0.5412(6) -0.1702(15) 0.079 Uiso 1 calc R .
C8 C 0.6271(6) 0.5094(4) 0.1223(13) 0.042(3) Uani 1 d . .
C6 C 0.5312(6) 0.4488(4) 0.1071(12) 0.044(3) Uani 1 d . .
H6A H 0.5407(6) 0.4483(4) 0.0028(12) 0.053 Uiso 1 calc R .
H6B H 0.4890(6) 0.4697(4) 0.1247(12) 0.053 Uiso 1 calc R .
C4 C 0.5641(7) 0.4197(5) 0.3992(13) 0.062(4) Uani 1 d . .
H4A H 0.6078(7) 0.3996(5) 0.3891(13) 0.074 Uiso 1 calc R .
H4B H 0.5516(7) 0.4213(5) 0.5021(13) 0.074 Uiso 1 calc R .
C40 C 0.6692(9) 0.4582(7) -0.2376(16) 0.096(5) Uani 1 d . .
H40A H 0.6650(9) 0.4251(7) -0.2678(16) 0.144 Uiso 1 calc R .
H40B H 0.7176(9) 0.4700(7) -0.2617(16) 0.144 Uiso 1 calc R .
H40C H 0.6325(9) 0.4772(7) -0.2871(16) 0.144 Uiso 1 calc R .
C7 C 0.5136(7) 0.3985(5) 0.1592(12) 0.057(4) Uani 1 d . .
H7A H 0.4690(7) 0.3871(5) 0.1116(12) 0.068 Uiso 1 calc R .
H7B H 0.5538(7) 0.3770(5) 0.1332(12) 0.068 Uiso 1 calc R .
C15 C 0.6997(9) 0.5869(6) -0.0055(21) 0.082(5) Uani 1 d . .
H15 H 0.7254(9) 0.6128(6) -0.0456(21) 0.098 Uiso 1 calc R .
C17 C 0.6295(7) 0.5520(5) 0.1852(16) 0.063(4) Uani 1 d . .
H17 H 0.6061(7) 0.5556(5) 0.2750(16) 0.075 Uiso 1 calc R .
O1 O 0.0032(8) 0.2500 0.1000(18) 0.089(5) Uani 1 d S .
C1 C 0.0662(10) 0.2500 0.0854(23) 0.061(5) Uani 1 d S .
O1S O 0.4848(23) 0.2500 0.7817(46) 0.280(17) Uani 1 d SU .
C1S C 0.4368(15) 0.2918(10) 0.7204(31) 0.177(11) Uani 1 d U .
H1S1 H 0.4650(15) 0.3081(10) 0.6450(31) 0.212 Uiso 1 calc R .
H1S2 H 0.4285(15) 0.3148(10) 0.7985(31) 0.212 Uiso 1 calc R .
C2S C 0.3587(16) 0.2774(9) 0.6538(30) 0.186(12) Uani 1 d U .
H2S1 H 0.3187(16) 0.2898(9) 0.7136(30) 0.224 Uiso 1 calc R .
H2S2 H 0.3533(16) 0.2898(9) 0.5553(30) 0.224 Uiso 1 calc R .
O2S O 0.0398(12) 0.2500 0.4663(31) 0.180(10) Uani 1 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'
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'
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
C1 Re1 C2 89.2(6) . 7_565 ?
C1 Re1 C2 89.2(6) . . ?
C2 Re1 C2 90.9(9) 7_565 . ?
C1 Re1 S1 92.2(5) . 7_565 ?
C2 Re1 S1 91.3(5) 7_565 7_565 ?
C2 Re1 S1 177.4(4) . 7_565 ?
C1 Re1 S1 92.2(5) . . ?
C2 Re1 S1 177.4(4) 7_565 . ?
C2 Re1 S1 91.3(5) . . ?
S1 Re1 S1 86.5(2) 7_565 . ?
C1 Re1 B1 168.0(8) . . ?
C2 Re1 B1 99.2(5) 7_565 . ?
C2 Re1 B1 99.2(5) . . ?
S1 Re1 B1 79.2(3) 7_565 . ?
S1 Re1 B1 79.2(3) . . ?
C11 S1 Re1 103.7(4) . . ?
C11 N11 C13 106.7(9) . . ?
C11 N11 B1 129.9(12) . . ?
C13 N11 B1 123.3(11) . . ?
C11 N12 C12 106.9(9) . . ?
C11 N12 C14 123.7(10) . . ?
C12 N12 C14 129.2(10) . . ?
O2 C2 Re1 178.6(13) . . ?
N11 C11 N12 109.4(9) . . ?
N11 C11 S1 126.7(9) . . ?
N12 C11 S1 123.7(8) . . ?
C9 O4 C40 119.4(11) . . ?
C8 N2 C6 115.1(9) . . ?
C8 N2 C5 115.1(10) . . ?
C6 N2 C5 110.0(9) . . ?
C12 C13 N11 109.7(10) . . ?
C3 N1 C4 118.7(10) . . ?
C3 N1 C7 127.3(10) . . ?
C4 N1 C7 113.7(9) . . ?
N2 C5 C4 108.8(11) . . ?
O3 C3 N1 123.7(12) . . ?
O3 C3 C12 119.7(12) . . ?
N1 C3 C12 116.4(10) . . ?
C13 C12 N12 107.3(10) . . ?
C13 C12 C3 131.3(11) . . ?
N12 C12 C3 120.8(10) . . ?
O4 C9 C10 121.9(12) . . ?
O4 C9 C8 116.5(10) . . ?
C10 C9 C8 121.6(12) . . ?
N11 B1 N11 110.4(14) 7_565 . ?
N11 B1 Re1 98.3(9) 7_565 . ?
N11 B1 Re1 98.3(9) . . ?
C15 C16 C17 117.9(15) . . ?
C15 C10 C9 118.9(14) . . ?
C17 C8 N2 125.3(12) . . ?
C17 C8 C9 116.4(12) . . ?
N2 C8 C9 118.2(10) . . ?
N2 C6 C7 110.5(9) . . ?
N1 C4 C5 110.7(10) . . ?
N1 C7 C6 110.2(11) . . ?
C10 C15 C16 120.9(15) . . ?
C8 C17 C16 124.2(15) . . ?
O1 C1 Re1 179.2(20) . . ?
C1S O1S C1S 96.5(33) 7_565 . ?
O1S C1S C2S 116.6(25) . . ?
C2S C2S C1S 104.6(14) 7_565 . ?
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 C1 1.89(2) . ?
Re1 C2 1.90(2) 7_565 ?
Re1 C2 1.90(2) . ?
Re1 S1 2.478(4) 7_565 ?
Re1 S1 2.478(4) . ?
Re1 B1 2.79(2) . ?
S1 C11 1.704(11) . ?
O2 C2 1.14(2) . ?
N11 C11 1.346(13) . ?
N11 C13 1.392(12) . ?
N11 B1 1.539(14) . ?
N12 C11 1.353(13) . ?
N12 C12 1.412(14) . ?
N12 C14 1.439(14) . ?
O4 C9 1.368(14) . ?
O4 C40 1.44(2) . ?
N2 C8 1.401(14) . ?
N2 C6 1.464(13) . ?
N2 C5 1.471(15) . ?
C13 C12 1.315(14) . ?
N1 C3 1.349(14) . ?
N1 C4 1.452(14) . ?
N1 C7 1.473(14) . ?
C5 C4 1.54(2) . ?
O3 C3 1.201(14) . ?
C3 C12 1.50(2) . ?
C9 C10 1.38(2) . ?
C9 C8 1.41(2) . ?
B1 N11 1.539(14) 7_565 ?
C16 C15 1.36(2) . ?
C16 C17 1.40(2) . ?
C10 C15 1.36(2) . ?
C8 C17 1.31(2) . ?
C6 C7 1.51(2) . ?
O1 C1 1.15(2) . ?
O1S C1S 1.55(3) 7_565 ?
O1S C1S 1.55(3) . ?
C1S C2S 1.59(3) . ?
C2S C2S 1.52(5) 7_565 ?
