#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179335 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/32/4323244.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_4323244
loop_
_publ_author_name
'António Paulo'
'K. Rajender Reddy'
'Ângela Domingos'
'Isabel Santos'
_publ_section_title
;
 Neutral trans-Dioxorhenium(V) Complexes with the Anionic
 Tetrakis(pyrazolyl)borate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6807
_journal_page_last               6813
_journal_paper_doi               10.1021/ic980422y
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C29 H38 B Cl6 N12 O2 Re'
_chemical_formula_weight         996.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                97.910(10)
_cell_angle_beta                 102.370(10)
_cell_angle_gamma                94.210(10)
_cell_formula_units_Z            2
_cell_length_a                   10.907(2)
_cell_length_b                   11.113(1)
_cell_length_c                   16.922(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      8.7
_cell_volume                     1973.2(5)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'MOLEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johonson, 1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer '
_diffrn_measurement_method       'ω/2θ 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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6567
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        1.9
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.531
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       irregular
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_obs          0.0311
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0413P)²+2.5717P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0787
_refine_ls_wR_factor_obs         0.0721
_reflns_number_observed          5555
_reflns_number_total             6199
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980422y_1.cif
_cod_data_source_block           COMPLEX5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+2.5717P] 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^)+(0.0413P)^2^+2.5717P] 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      'P 1'
_cod_database_code               4323244
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Re Re 0.15360(2) 0.17203(2) 0.227655(12) 0.03175(8) Uani 1 d . .
O1 O 0.2465(3) 0.3141(3) 0.2578(2) 0.0376(8) Uani 1 d . .
O2 O 0.0767(3) 0.0227(3) 0.2037(2) 0.0413(8) Uani 1 d . .
N1 N -0.0013(4) 0.2483(4) 0.2647(2) 0.0367(9) Uani 1 d . .
N2 N 0.0785(4) 0.2061(4) 0.1085(2) 0.0369(9) Uani 1 d . .
N3 N -0.2750(4) 0.3505(4) 0.0762(3) 0.0590(13) Uani 1 d . .
N4 N 0.0439(5) 0.5853(4) 0.2327(3) 0.0613(14) Uani 1 d . .
N5 N 0.3148(4) 0.0993(3) 0.1892(2) 0.0349(9) Uani 1 d . .
N6 N 0.2322(4) 0.1289(4) 0.3486(2) 0.0361(9) Uani 1 d . .
N7 N 0.6258(4) -0.0294(4) 0.1079(3) 0.0567(13) Uani 1 d . .
N8 N 0.3901(5) 0.0415(5) 0.5796(3) 0.0659(15) Uani 1 d . .
N11 N -0.0730(4) 0.3272(4) 0.2250(2) 0.0368(9) Uani 1 d . .
N21 N -0.0081(4) 0.2848(4) 0.0883(2) 0.0349(9) Uani 1 d . .
N31 N -0.1672(4) 0.4283(4) 0.1063(3) 0.0404(10) Uani 1 d . .
N41 N 0.0567(4) 0.4902(4) 0.1768(3) 0.0391(10) Uani 1 d . .
C1 C 0.3149(5) -0.0180(5) 0.1568(3) 0.0421(12) Uani 1 d . .
H1 H 0.2438(5) -0.0718(5) 0.1534(3) 0.059(6) Uiso 1 calc R .
C2 C 0.4133(5) -0.0629(5) 0.1287(4) 0.0492(14) Uani 1 d . .
H2 H 0.4065(5) -0.1449(5) 0.1059(4) 0.059(6) Uiso 1 calc R .
C3 C 0.5245(5) 0.0118(5) 0.1335(3) 0.0409(12) Uani 1 d . .
C4 C 0.5245(5) 0.1341(5) 0.1672(4) 0.0475(13) Uani 1 d . .
H4 H 0.5950(5) 0.1893(5) 0.1720(4) 0.059(6) Uiso 1 calc R .
C5 C 0.4222(5) 0.1726(5) 0.1931(4) 0.0472(13) Uani 1 d . .
H5 H 0.4259(5) 0.2547(5) 0.2149(4) 0.059(6) Uiso 1 calc R .
C6 C 0.3282(5) 0.1998(5) 0.4019(3) 0.0475(13) Uani 1 d . .
H6 H 0.3598(5) 0.2707(5) 0.3863(3) 0.059(6) Uiso 1 calc R .
C7 C 0.3825(5) 0.1745(5) 0.4779(3) 0.0527(15) Uani 1 d . .
H7 H 0.4487(5) 0.2277(5) 0.5117(3) 0.059(6) Uiso 1 calc R .
C8 C 0.3396(5) 0.0703(5) 0.5048(3) 0.0475(13) Uani 1 d . .
C9 C 0.2409(6) -0.0032(5) 0.4488(4) 0.056(2) Uani 1 d . .
H9 H 0.2079(6) -0.0751(5) 0.4625(4) 0.059(6) Uiso 1 calc R .
C10 C 0.1921(5) 0.0288(5) 0.3745(3) 0.0485(13) Uani 1 d . .
H10 H 0.1262(5) -0.0232(5) 0.3394(3) 0.059(6) Uiso 1 calc R .
C11 C -0.1605(5) 0.3580(5) 0.2666(3) 0.0462(13) Uani 1 d . .
H11 H -0.2204(5) 0.4115(5) 0.2526(3) 0.060(5) Uiso 1 calc R .
C12 C -0.1476(6) 0.2983(6) 0.3327(4) 0.0542(15) Uani 1 d . .
H12 H -0.1956(6) 0.3028(6) 0.3720(4) 0.060(5) Uiso 1 calc R .
C13 C -0.0489(5) 0.2308(5) 0.3287(3) 0.0494(14) Uani 1 d . .
H13 H -0.0191(5) 0.1794(5) 0.3658(3) 0.060(5) Uiso 1 calc R .
C21 C -0.0451(5) 0.2709(5) 0.0066(3) 0.0435(12) Uani 1 d . .
H21 H -0.1033(5) 0.3152(5) -0.0224(3) 0.060(5) Uiso 1 calc R .
C22 C 0.0160(5) 0.1809(5) -0.0279(3) 0.0487(14) Uani 1 d . .
H22 H 0.0080(5) 0.1520(5) -0.0832(3) 0.060(5) Uiso 1 calc R .
C23 C 0.0923(5) 0.1434(5) 0.0388(3) 0.0417(12) Uani 1 d . .
H23 H 0.1459(5) 0.0826(5) 0.0352(3) 0.060(5) Uiso 1 calc R .
C31 C -0.1816(5) 0.5360(5) 0.0793(3) 0.0462(13) Uani 1 d . .
H31 H -0.1211(5) 0.6034(5) 0.0919(3) 0.060(5) Uiso 1 calc R .
C33 C -0.3521(5) 0.4133(6) 0.0311(4) 0.061(2) Uani 1 d . .
H33 H -0.4336(5) 0.3824(6) 0.0026(4) 0.060(5) Uiso 1 calc R .
C32 C -0.2989(5) 0.5300(5) 0.0306(4) 0.0538(15) Uani 1 d . .
H32 H -0.3352(5) 0.5903(5) 0.0033(4) 0.060(5) Uiso 1 calc R .
C41 C 0.1540(5) 0.5172(5) 0.1434(4) 0.0495(14) Uani 1 d . .
H41 H 0.1810(5) 0.4660(5) 0.1038(4) 0.060(5) Uiso 1 calc R .
C43 C 0.1347(7) 0.6708(6) 0.2322(4) 0.073(2) Uani 1 d . .
H43 H 0.1485(7) 0.7474(6) 0.2646(4) 0.060(5) Uiso 1 calc R .
C42 C 0.2063(6) 0.6322(6) 0.1775(4) 0.061(2) Uani 1 d . .
H42 H 0.2753(6) 0.6754(6) 0.1664(4) 0.060(5) Uiso 1 calc R .
C71 C 0.7419(5) 0.0495(6) 0.1171(5) 0.068(2) Uani 1 d . .
H71A H 0.8020(5) 0.0039(6) 0.0954(5) 0.117(9) Uiso 1 calc R .
H71B H 0.7759(5) 0.0802(6) 0.1741(5) 0.117(9) Uiso 1 calc R .
H71C H 0.7245(5) 0.1167(6) 0.0878(5) 0.117(9) Uiso 1 calc R .
C72 C 0.6193(7) -0.1526(6) 0.0677(5) 0.079(2) Uani 1 d . .
H72A H 0.6985(7) -0.1665(6) 0.0538(5) 0.117(9) Uiso 1 calc R .
H72B H 0.5534(7) -0.1660(6) 0.0187(5) 0.117(9) Uiso 1 calc R .
H72C H 0.6016(7) -0.2080(6) 0.1037(5) 0.117(9) Uiso 1 calc R .
C81 C 0.4911(7) 0.1200(7) 0.6370(4) 0.079(2) Uani 1 d . .
H81A H 0.5141(7) 0.0847(7) 0.6861(4) 0.117(9) Uiso 1 calc R .
H81B H 0.4635(7) 0.1989(7) 0.6500(4) 0.117(9) Uiso 1 calc R .
H81C H 0.5628(7) 0.1285(7) 0.6130(4) 0.117(9) Uiso 1 calc R .
C82 C 0.3382(8) -0.0649(7) 0.6070(4) 0.084(2) Uani 1 d . .
H82A H 0.3855(8) -0.0709(7) 0.6609(4) 0.117(9) Uiso 1 calc R .
H82B H 0.3433(8) -0.1370(7) 0.5699(4) 0.117(9) Uiso 1 calc R .
H82C H 0.2516(8) -0.0575(7) 0.6084(4) 0.117(9) Uiso 1 calc R .
B B -0.0460(5) 0.3828(5) 0.1510(4) 0.0357(12) Uani 1 d . .
Cl1 Cl 0.5300(2) 0.5292(3) 0.1970(2) 0.1313(10) Uani 1 d . .
Cl2 Cl 0.5674(2) 0.4848(3) 0.3621(2) 0.1273(10) Uani 1 d . .
Cl3 Cl 0.1546(3) 0.4336(3) 0.4847(2) 0.1369(10) Uani 1 d . .
Cl4 Cl 0.2817(3) 0.6432(3) 0.4425(2) 0.1484(12) Uani 1 d . .
Cl5 Cl 0.9394(4) -0.1924(5) 0.4211(3) 0.200(2) Uani 1 d . .
Cl6 Cl 0.8200(6) -0.1657(4) 0.2650(3) 0.232(3) Uani 1 d . .
C1S C 0.4623(7) 0.5258(6) 0.2806(5) 0.074(2) Uani 1 d . .
H1S1 H 0.4373(7) 0.6058(6) 0.2968(5) 0.150(17) Uiso 1 calc R .
H1S2 H 0.3873(7) 0.4676(6) 0.2654(5) 0.150(17) Uiso 1 calc R .
C2S C 0.1750(11) 0.5135(8) 0.4089(5) 0.118(4) Uani 1 d . .
H2S1 H 0.0941(11) 0.5372(8) 0.3829(5) 0.150(17) Uiso 1 calc R .
H2S2 H 0.2040(11) 0.4605(8) 0.3677(5) 0.150(17) Uiso 1 calc R .
C3S C 0.8450(10) -0.2665(9) 0.3321(9) 0.138(4) Uani 1 d . .
H3S1 H 0.7653(10) -0.2985(9) 0.3418(9) 0.150(17) Uiso 1 calc R .
H3S2 H 0.8851(10) -0.3343(9) 0.3100(9) 0.150(17) Uiso 1 calc R .
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'
Re Re -1.0185 7.2310 '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'
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
O2 Re O1 173.11(15) . . ?
O2 Re N2 91.1(2) . . ?
O1 Re N2 94.0(2) . . ?
O2 Re N1 93.7(2) . . ?
O1 Re N1 91.06(15) . . ?
N2 Re N1 88.5(2) . . ?
O2 Re N5 87.94(15) . . ?
O1 Re N5 87.34(15) . . ?
N2 Re N5 90.94(15) . . ?
N1 Re N5 178.24(15) . . ?
O2 Re N6 87.0(2) . . ?
O1 Re N6 87.82(15) . . ?
N2 Re N6 177.6(2) . . ?
N1 Re N6 93.2(2) . . ?
N5 Re N6 87.49(15) . . ?
C13 N1 N11 106.4(4) . . ?
C13 N1 Re 128.6(4) . . ?
N11 N1 Re 125.1(3) . . ?
C23 N2 N21 106.9(4) . . ?
C23 N2 Re 126.8(3) . . ?
N21 N2 Re 125.7(3) . . ?
C33 N3 N31 104.6(5) . . ?
C43 N4 N41 105.1(5) . . ?
C1 N5 C5 115.0(4) . . ?
C1 N5 Re 123.5(3) . . ?
C5 N5 Re 121.4(3) . . ?
C10 N6 C6 114.8(4) . . ?
C10 N6 Re 122.8(3) . . ?
C6 N6 Re 122.4(3) . . ?
C3 N7 C72 120.3(5) . . ?
C3 N7 C71 121.9(5) . . ?
C72 N7 C71 117.7(5) . . ?
C8 N8 C81 121.5(5) . . ?
C8 N8 C82 121.0(6) . . ?
C81 N8 C82 117.4(5) . . ?
C11 N11 N1 108.6(4) . . ?
C11 N11 B 126.0(4) . . ?
N1 N11 B 125.1(4) . . ?
C21 N21 N2 108.8(4) . . ?
C21 N21 B 126.6(4) . . ?
N2 N21 B 124.3(4) . . ?
C31 N31 N3 110.0(4) . . ?
C31 N31 B 128.4(4) . . ?
N3 N31 B 120.8(4) . . ?
C41 N41 N4 110.4(4) . . ?
C41 N41 B 129.4(5) . . ?
N4 N41 B 119.3(4) . . ?
N5 C1 C2 123.8(5) . . ?
C1 C2 C3 121.3(5) . . ?
N7 C3 C4 121.7(5) . . ?
N7 C3 C2 123.4(5) . . ?
C4 C3 C2 114.9(5) . . ?
C5 C4 C3 120.5(5) . . ?
C4 C5 N5 124.5(5) . . ?
N6 C6 C7 124.3(5) . . ?
C6 C7 C8 120.6(5) . . ?
N8 C8 C7 122.8(5) . . ?
N8 C8 C9 122.5(5) . . ?
C7 C8 C9 114.7(5) . . ?
C10 C9 C8 121.0(5) . . ?
N6 C10 C9 124.6(5) . . ?
N11 C11 C12 109.0(5) . . ?
C13 C12 C11 105.2(5) . . ?
N1 C13 C12 110.9(5) . . ?
N21 C21 C22 109.5(5) . . ?
C21 C22 C23 103.9(5) . . ?
N2 C23 C22 110.9(5) . . ?
N31 C31 C32 108.7(5) . . ?
N3 C33 C32 112.7(5) . . ?
C31 C32 C33 103.9(5) . . ?
N41 C41 C42 108.2(6) . . ?
N4 C43 C42 111.5(6) . . ?
C41 C42 C43 104.8(6) . . ?
N41 B N31 108.3(4) . . ?
N41 B N11 112.1(4) . . ?
N31 B N11 108.9(4) . . ?
N41 B N21 109.5(4) . . ?
N31 B N21 106.8(4) . . ?
N11 B N21 111.0(4) . . ?
Cl2 C1S Cl1 110.9(4) . . ?
Cl3 C2S Cl4 113.8(5) . . ?
Cl5 C3S Cl6 108.3(6) . . ?
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
Re O2 1.756(3) . ?
Re O1 1.761(3) . ?
Re N2 2.104(4) . ?
Re N1 2.118(4) . ?
Re N5 2.173(4) . ?
Re N6 2.174(4) . ?
N1 C13 1.328(6) . ?
N1 N11 1.367(5) . ?
N2 C23 1.329(6) . ?
N2 N21 1.356(5) . ?
N3 C33 1.317(8) . ?
N3 N31 1.365(6) . ?
N4 C43 1.325(8) . ?
N4 N41 1.353(6) . ?
N5 C1 1.344(6) . ?
N5 C5 1.361(6) . ?
N6 C10 1.330(7) . ?
N6 C6 1.346(6) . ?
N7 C3 1.358(7) . ?
N7 C72 1.432(7) . ?
N7 C71 1.453(7) . ?
N8 C8 1.359(7) . ?
N8 C81 1.444(8) . ?
N8 C82 1.448(9) . ?
N11 C11 1.339(6) . ?
N11 B 1.543(7) . ?
N21 C21 1.338(6) . ?
N21 B 1.556(7) . ?
N31 C31 1.346(7) . ?
N31 B 1.534(7) . ?
N41 C41 1.339(7) . ?
N41 B 1.523(7) . ?
C1 C2 1.364(7) . ?
C2 C3 1.400(7) . ?
C3 C4 1.399(7) . ?
C4 C5 1.359(7) . ?
C6 C7 1.371(8) . ?
C7 C8 1.387(8) . ?
C8 C9 1.394(8) . ?
C9 C10 1.362(8) . ?
C11 C12 1.365(8) . ?
C12 C13 1.364(8) . ?
C21 C22 1.374(8) . ?
C22 C23 1.385(7) . ?
C31 C32 1.357(8) . ?
C33 C32 1.384(8) . ?
C41 C42 1.357(8) . ?
C43 C42 1.378(10) . ?
Cl1 C1S 1.733(8) . ?
Cl2 C1S 1.731(7) . ?
Cl3 C2S 1.700(9) . ?
Cl4 C2S 1.732(10) . ?
Cl5 C3S 1.695(13) . ?
Cl6 C3S 1.698(12) . ?
