#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:16:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179782 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/78/7007825.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_7007825
loop_
_publ_author_name
'Moura, Carolina'
'Vítor, Rute F'
'Maria, Leonor'
'Paulo, António'
'Santos, Isabel C.'
'Santos, Isabel'
_publ_section_title
;
 Rhenium(V) oxocomplexes with novel pyrazolyl-based N4- and N3S-donor
 chelators.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5630
_journal_page_last               5640
_journal_paper_doi               10.1039/b611034g
_journal_year                    2006
_chemical_formula_moiety         'C12 H25 N5 O2 Re, C24 H20 B'
_chemical_formula_sum            'C36 H45 B N5 O2 Re'
_chemical_formula_weight         776.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.285(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.101(2)
_cell_length_b                   14.3993(15)
_cell_length_c                   19.975(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     3459.6(8)
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_collection       'CAD4 Software (Enraf-Nonius,1994) '
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    ORTEP3(Farrugia,1997
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       ω-2θ
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.1187
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7102
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.75
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_T_max  0.4155
_exptl_absorpt_correction_T_min  0.4155
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'North A.C.T.,Phillips D.C.,Mathews F.S.(1968) Acta.Cryst.A24,351'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1474
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0310P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                3812
_reflns_number_total             6767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b611034g.txt
_cod_data_source_block           11
_cod_original_cell_volume        3459.6(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7007825
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_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
Re1 Re 0.53494(3) 0.13521(3) 0.92000(2) 0.03868(13) Uani 1 1 d . . .
O1 O 0.4830(6) 0.1038(4) 0.9929(3) 0.0530(19) Uani 1 1 d . . .
O2 O 0.5339(6) 0.1640(4) 0.8246(3) 0.0502(19) Uani 1 1 d . . .
N1 N 0.5468(7) 0.2784(5) 0.9365(4) 0.043(2) Uani 1 1 d . . .
N2 N 0.6391(8) 0.3159(6) 0.9717(4) 0.053(3) Uani 1 1 d . . .
N3 N 0.6933(7) 0.1258(6) 0.9361(4) 0.053(2) Uani 1 1 d . . .
N4 N 0.5477(7) -0.0033(5) 0.8886(4) 0.048(2) Uani 1 1 d . . .
H4 H 0.5447 -0.0396 0.9257 0.057 Uiso 1 1 calc R . .
N5 N 0.3561(6) 0.1072(5) 0.8729(4) 0.055(2) Uani 1 1 d . . .
H5A H 0.3067 0.1275 0.9001 0.066 Uiso 1 1 calc R . .
H5B H 0.3427 0.1358 0.8328 0.066 Uiso 1 1 calc R . .
C1 C 0.7206(9) 0.2581(8) 1.0094(6) 0.069(4) Uani 1 1 d . . .
H1A H 0.6851 0.2234 1.0428 0.083 Uiso 1 1 calc R . .
H1B H 0.7773 0.2972 1.0331 0.083 Uiso 1 1 calc R . .
C2 C 0.7747(10) 0.1911(8) 0.9650(7) 0.080(4) Uani 1 1 d . . .
H2A H 0.8059 0.2249 0.9295 0.096 Uiso 1 1 calc R . .
H2B H 0.8346 0.1584 0.9914 0.096 Uiso 1 1 calc R . .
C3 C 0.7383(9) 0.0348(8) 0.9175(6) 0.066(4) Uani 1 1 d . . .
H3A H 0.7523 -0.0033 0.9576 0.079 Uiso 1 1 calc R . .
H3B H 0.8087 0.0444 0.8995 0.079 Uiso 1 1 calc R . .
C4 C 0.6604(9) -0.0158(8) 0.8662(5) 0.055(3) Uani 1 1 d . . .
H4A H 0.6632 0.0104 0.8217 0.066 Uiso 1 1 calc R . .
H4B H 0.6795 -0.0812 0.8650 0.066 Uiso 1 1 calc R . .
C5 C 0.4536(9) -0.0309(7) 0.8391(6) 0.062(3) Uani 1 1 d . . .
H5C H 0.4505 -0.0979 0.8347 0.074 Uiso 1 1 calc R . .
H5D H 0.4622 -0.0043 0.7953 0.074 Uiso 1 1 calc R . .
C6 C 0.3489(9) 0.0053(7) 0.8648(6) 0.062(3) Uani 1 1 d . . .
H6A H 0.2850 -0.0105 0.8333 0.075 Uiso 1 1 calc R . .
H6B H 0.3396 -0.0234 0.9078 0.075 Uiso 1 1 calc R . .
C7 C 0.6144(10) 0.2183(8) 0.7964(5) 0.081(4) Uani 1 1 d . . .
H7A H 0.6038 0.2129 0.7482 0.121 Uiso 1 1 calc R . .
H7B H 0.6874 0.1968 0.8129 0.121 Uiso 1 1 calc R . .
H7C H 0.6065 0.2821 0.8090 0.121 Uiso 1 1 calc R . .
C8 C 0.3812(9) 0.3394(7) 0.8689(6) 0.071(4) Uani 1 1 d . . .
H8A H 0.3337 0.3005 0.8923 0.106 Uiso 1 1 calc R . .
H8B H 0.3934 0.3108 0.8269 0.106 Uiso 1 1 calc R . .
H8C H 0.3465 0.3988 0.8604 0.106 Uiso 1 1 calc R . .
C9 C 0.7274(11) 0.4693(8) 1.0021(7) 0.094(5) Uani 1 1 d . . .
H9A H 0.7699 0.4344 1.0369 0.141 Uiso 1 1 calc R . .
H9B H 0.6939 0.5217 1.0216 0.141 Uiso 1 1 calc R . .
H9C H 0.7756 0.4905 0.9701 0.141 Uiso 1 1 calc R . .
C11 C 0.4878(8) 0.3517(7) 0.9101(5) 0.049(3) Uani 1 1 d . . .
C12 C 0.5424(11) 0.4324(7) 0.9279(6) 0.056(3) Uani 1 1 d . . .
H12 H 0.5188 0.4921 0.9156 0.067 Uiso 1 1 calc R . .
C13 C 0.6390(10) 0.4090(8) 0.9673(5) 0.054(3) Uani 1 1 d . . .
C21 C 0.5791(9) 0.6746(6) 0.8132(5) 0.046(3) Uani 1 1 d . . .
C22 C 0.5559(9) 0.7110(7) 0.8751(5) 0.047(3) Uani 1 1 d . . .
H22 H 0.4829 0.7271 0.8805 0.056 Uiso 1 1 calc R . .
C23 C 0.6375(11) 0.7239(7) 0.9287(6) 0.071(4) Uani 1 1 d . . .
H23 H 0.6189 0.7504 0.9684 0.085 Uiso 1 1 calc R . .
C24 C 0.7437(10) 0.6983(8) 0.9239(6) 0.069(4) Uani 1 1 d . . .
H24 H 0.7978 0.7073 0.9602 0.082 Uiso 1 1 calc R . .
C25 C 0.7715(10) 0.6592(9) 0.8656(6) 0.078(4) Uani 1 1 d . . .
H25 H 0.8439 0.6394 0.8623 0.094 Uiso 1 1 calc R . .
C26 C 0.6901(9) 0.6496(8) 0.8116(5) 0.061(3) Uani 1 1 d . . .
H26 H 0.7108 0.6250 0.7718 0.073 Uiso 1 1 calc R . .
C31 C 0.5010(8) 0.5817(8) 0.6990(5) 0.048(3) Uani 1 1 d . . .
C32 C 0.5462(10) 0.4981(8) 0.7215(6) 0.067(4) Uani 1 1 d . . .
H32 H 0.5752 0.4934 0.7664 0.080 Uiso 1 1 calc R . .
C33 C 0.5509(12) 0.4201(8) 0.6807(8) 0.090(5) Uani 1 1 d . . .
H33 H 0.5846 0.3659 0.6981 0.108 Uiso 1 1 calc R . .
C34 C 0.5052(13) 0.4237(11) 0.6141(7) 0.091(5) Uani 1 1 d . . .
H34 H 0.5061 0.3719 0.5864 0.110 Uiso 1 1 calc R . .
C35 C 0.4595(10) 0.5037(11) 0.5906(6) 0.074(4) Uani 1 1 d . . .
H35 H 0.4270 0.5066 0.5462 0.088 Uiso 1 1 calc R . .
C36 C 0.4593(9) 0.5827(8) 0.6310(6) 0.062(3) Uani 1 1 d . . .
H36 H 0.4306 0.6378 0.6120 0.074 Uiso 1 1 calc R . .
C41 C 0.3623(9) 0.6710(8) 0.7702(5) 0.052(3) Uani 1 1 d . . .
C42 C 0.3144(10) 0.5879(9) 0.7874(6) 0.064(3) Uani 1 1 d . . .
H42 H 0.3546 0.5336 0.7829 0.077 Uiso 1 1 calc R . .
C43 C 0.2115(11) 0.5800(11) 0.8105(6) 0.084(5) Uani 1 1 d . . .
H43 H 0.1825 0.5223 0.8199 0.101 Uiso 1 1 calc R . .
C44 C 0.1530(11) 0.6608(12) 0.8193(6) 0.086(5) Uani 1 1 d . . .
H44 H 0.0839 0.6574 0.8353 0.104 Uiso 1 1 calc R . .
C45 C 0.1939(10) 0.7427(11) 0.8051(6) 0.078(4) Uani 1 1 d . . .
H45 H 0.1543 0.7967 0.8117 0.094 Uiso 1 1 calc R . .
C46 C 0.2993(9) 0.7477(8) 0.7796(5) 0.060(3) Uani 1 1 d . . .
H46 H 0.3263 0.8057 0.7689 0.072 Uiso 1 1 calc R . .
C51 C 0.5066(9) 0.7696(7) 0.7034(5) 0.046(3) Uani 1 1 d . . .
C52 C 0.6033(9) 0.8219(7) 0.7103(6) 0.054(3) Uani 1 1 d . . .
H52 H 0.6604 0.8043 0.7429 0.065 Uiso 1 1 calc R . .
C53 C 0.6193(11) 0.8998(8) 0.6707(7) 0.073(4) Uani 1 1 d . . .
H53 H 0.6852 0.9334 0.6776 0.087 Uiso 1 1 calc R . .
C54 C 0.5363(13) 0.9266(8) 0.6212(6) 0.078(4) Uani 1 1 d . . .
H54 H 0.5456 0.9781 0.5943 0.093 Uiso 1 1 calc R . .
C55 C 0.4414(11) 0.8763(9) 0.6128(7) 0.082(4) Uani 1 1 d . . .
H55 H 0.3855 0.8927 0.5792 0.098 Uiso 1 1 calc R . .
C56 C 0.4267(10) 0.8015(8) 0.6532(6) 0.069(4) Uani 1 1 d . . .
H56 H 0.3592 0.7700 0.6468 0.083 Uiso 1 1 calc R . .
B1 B 0.4875(10) 0.6746(8) 0.7464(6) 0.045(3) Uani 1 1 d . . .
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'
Re Re -1.0185 7.2310 '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'
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
O1 Re1 N3 107.1(3) . . ?
O1 Re1 O2 157.8(3) . . ?
N3 Re1 O2 94.5(3) . . ?
O1 Re1 N1 98.7(3) . . ?
N3 Re1 N1 89.6(4) . . ?
O2 Re1 N1 86.4(3) . . ?
O1 Re1 N4 92.8(3) . . ?
N3 Re1 N4 83.0(3) . . ?
O2 Re1 N4 84.4(3) . . ?
N1 Re1 N4 167.7(3) . . ?
O1 Re1 N5 83.4(3) . . ?
N3 Re1 N5 159.6(3) . . ?
O2 Re1 N5 74.5(3) . . ?
N1 Re1 N5 106.4(3) . . ?
N4 Re1 N5 78.9(3) . . ?
C7 O2 Re1 125.2(6) . . ?
C11 N1 N2 105.1(8) . . ?
C11 N1 Re1 133.3(7) . . ?
N2 N1 Re1 120.7(7) . . ?
C13 N2 N1 111.5(10) . . ?
C13 N2 C1 127.4(11) . . ?
N1 N2 C1 121.1(9) . . ?
C2 N3 C3 115.1(9) . . ?
C2 N3 Re1 130.7(7) . . ?
C3 N3 Re1 114.2(7) . . ?
C5 N4 C4 115.4(8) . . ?
C5 N4 Re1 112.2(6) . . ?
C4 N4 Re1 107.7(6) . . ?
C6 N5 Re1 105.1(6) . . ?
N2 C1 C2 112.3(10) . . ?
N3 C2 C1 109.4(10) . . ?
N3 C3 C4 112.3(9) . . ?
N4 C4 C3 105.2(8) . . ?
N4 C5 C6 107.0(9) . . ?
N5 C6 C5 109.7(9) . . ?
N1 C11 C12 110.1(9) . . ?
N1 C11 C8 121.4(9) . . ?
C12 C11 C8 128.4(10) . . ?
C11 C12 C13 107.2(10) . . ?
N2 C13 C12 106.0(11) . . ?
N2 C13 C9 123.7(12) . . ?
C12 C13 C9 130.2(12) . . ?
C26 C21 C22 113.8(10) . . ?
C26 C21 B1 123.3(9) . . ?
C22 C21 B1 122.5(9) . . ?
C23 C22 C21 122.5(10) . . ?
C24 C23 C22 120.8(12) . . ?
C23 C24 C25 119.8(12) . . ?
C24 C25 C26 118.9(12) . . ?
C25 C26 C21 124.1(11) . . ?
C32 C31 C36 114.4(11) . . ?
C32 C31 B1 125.5(10) . . ?
C36 C31 B1 120.0(10) . . ?
C31 C32 C33 123.8(12) . . ?
C34 C33 C32 119.6(13) . . ?
C35 C34 C33 118.4(14) . . ?
C34 C35 C36 121.6(13) . . ?
C35 C36 C31 122.1(12) . . ?
C46 C41 C42 114.1(10) . . ?
C46 C41 B1 124.2(10) . . ?
C42 C41 B1 121.5(10) . . ?
C43 C42 C41 124.7(13) . . ?
C42 C43 C44 117.9(14) . . ?
C45 C44 C43 121.0(14) . . ?
C44 C45 C46 119.4(14) . . ?
C41 C46 C45 122.9(12) . . ?
C52 C51 C56 113.9(10) . . ?
C52 C51 B1 124.4(10) . . ?
C56 C51 B1 121.6(10) . . ?
C51 C52 C53 123.1(12) . . ?
C54 C53 C52 119.6(12) . . ?
C55 C54 C53 118.6(12) . . ?
C54 C55 C56 120.8(12) . . ?
C55 C56 C51 124.0(12) . . ?
C41 B1 C21 109.1(9) . . ?
C41 B1 C51 111.4(9) . . ?
C21 B1 C51 107.7(8) . . ?
C41 B1 C31 107.0(8) . . ?
C21 B1 C31 111.4(9) . . ?
C51 B1 C31 110.3(8) . . ?
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 O1 1.708(6) . ?
Re1 N3 1.913(8) . ?
Re1 O2 1.948(6) . ?
Re1 N1 2.090(8) . ?
Re1 N4 2.101(8) . ?
Re1 N5 2.299(8) . ?
O2 C7 1.413(11) . ?
N1 C11 1.349(11) . ?
N1 N2 1.364(11) . ?
N2 C13 1.343(12) . ?
N2 C1 1.439(12) . ?
N3 C2 1.437(12) . ?
N3 C3 1.482(12) . ?
N4 C5 1.479(12) . ?
N4 C4 1.492(12) . ?
N5 C6 1.478(11) . ?
C1 C2 1.508(15) . ?
C3 C4 1.503(14) . ?
C5 C6 1.511(14) . ?
C8 C11 1.464(13) . ?
C9 C13 1.489(15) . ?
C11 C12 1.365(13) . ?
C12 C13 1.378(15) . ?
C21 C26 1.394(14) . ?
C21 C22 1.400(13) . ?
C21 B1 1.639(15) . ?
C22 C23 1.388(14) . ?
C23 C24 1.350(15) . ?
C24 C25 1.369(15) . ?
C25 C26 1.386(14) . ?
C31 C32 1.376(13) . ?
C31 C36 1.398(14) . ?
C31 B1 1.656(15) . ?
C32 C33 1.392(15) . ?
C33 C34 1.385(17) . ?
C34 C35 1.340(17) . ?
C35 C36 1.394(15) . ?
C41 C46 1.367(14) . ?
C41 C42 1.389(14) . ?
C41 B1 1.639(15) . ?
C42 C43 1.379(15) . ?
C43 C44 1.383(17) . ?
C44 C45 1.322(16) . ?
C45 C46 1.425(15) . ?
C51 C52 1.386(13) . ?
C51 C56 1.392(14) . ?
C51 B1 1.645(15) . ?
C52 C53 1.399(14) . ?
C53 C54 1.386(16) . ?
C54 C55 1.352(16) . ?
C55 C56 1.370(15) . ?
