#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:21:14 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179786 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/82/7008296.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_7008296
loop_
_publ_author_name
'Mosch-Zanetti, Nadia C'
'Sachse, Anna'
'Pfoh, Roland'
'Vidovic, Denis'
'Magull, Jorg'
_publ_section_title
;
 Rhenium oxo compounds containing eta2-pyrazolate ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2124
_journal_page_last               2129
_journal_paper_doi               10.1039/b501025j
_journal_year                    2005
_chemical_formula_sum            'C12 H21 N2 O3 Re'
_chemical_formula_weight         427.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_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                 97.253(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2384(4)
_cell_length_b                   9.0653(4)
_cell_length_c                   14.5734(6)
_cell_measurement_temperature    133(2)
_cell_volume                     1472.85(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25266
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    8.253
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0160
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0180P)²+2.7477P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0393
_reflns_number_gt                2460
_reflns_number_total             2524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b501025j.txt
_cod_data_source_block           as3
_cod_database_code               7008296
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
Re Re 0.912249(10) 0.562459(13) 0.604925(8) 0.02547(6) Uani 1 1 d . . .
O1 O 1.0140(2) 0.4638(3) 0.6762(2) 0.0486(7) Uani 1 1 d . . .
O2 O 0.9917(2) 0.6534(3) 0.53025(17) 0.0369(5) Uani 1 1 d . . .
O3 O 0.8558(2) 0.6912(3) 0.67226(17) 0.0436(6) Uani 1 1 d . . .
N1 N 0.7587(2) 0.5173(3) 0.51081(16) 0.0205(5) Uani 1 1 d . . .
N2 N 0.7928(2) 0.3993(3) 0.56858(16) 0.0194(5) Uani 1 1 d . . .
C1 C 0.6900(2) 0.4672(3) 0.43593(19) 0.0182(6) Uani 1 1 d . . .
C2 C 0.6772(2) 0.3124(3) 0.44628(19) 0.0194(6) Uani 1 1 d . . .
C3 C 0.7467(2) 0.2731(3) 0.52915(19) 0.0191(6) Uani 1 1 d . . .
C4 C 0.6355(3) 0.5727(3) 0.3616(2) 0.0228(6) Uani 1 1 d . . .
C5 C 0.6868(3) 0.7277(3) 0.3818(2) 0.0357(8) Uani 1 1 d . . .
H5A H 0.7737 0.7260 0.3806 0.054 Uiso 1 1 calc R . .
H5B H 0.6696 0.7597 0.4430 0.054 Uiso 1 1 calc R . .
H5C H 0.6498 0.7966 0.3348 0.054 Uiso 1 1 calc R . .
C6 C 0.6642(3) 0.5241(4) 0.2661(2) 0.0311(7) Uani 1 1 d . . .
H6A H 0.7513 0.5181 0.2666 0.047 Uiso 1 1 calc R . .
H6B H 0.6311 0.5959 0.2195 0.047 Uiso 1 1 calc R . .
H6C H 0.6285 0.4270 0.2511 0.047 Uiso 1 1 calc R . .
C7 C 0.4992(3) 0.5775(4) 0.3640(2) 0.0314(7) Uani 1 1 d . . .
H7A H 0.4622 0.6435 0.3153 0.047 Uiso 1 1 calc R . .
H7B H 0.4826 0.6139 0.4244 0.047 Uiso 1 1 calc R . .
H7C H 0.4659 0.4780 0.3538 0.047 Uiso 1 1 calc R . .
C8 C 0.6014(3) 0.2119(4) 0.3809(2) 0.0299(7) Uani 1 1 d . . .
H8A H 0.6224 0.2250 0.3182 0.045 Uiso 1 1 calc R . .
H8B H 0.5165 0.2359 0.3817 0.045 Uiso 1 1 calc R . .
H8C H 0.6158 0.1092 0.4003 0.045 Uiso 1 1 calc R . .
C9 C 0.7757(3) 0.1252(3) 0.5742(2) 0.0262(6) Uani 1 1 d . . .
C10 C 0.8406(3) 0.0313(4) 0.5071(3) 0.0436(9) Uani 1 1 d . . .
H10A H 0.8620 -0.0648 0.5354 0.065 Uiso 1 1 calc R . .
H10B H 0.9136 0.0823 0.4943 0.065 Uiso 1 1 calc R . .
H10C H 0.7874 0.0168 0.4492 0.065 Uiso 1 1 calc R . .
C11 C 0.8578(4) 0.1450(4) 0.6648(3) 0.0526(11) Uani 1 1 d . . .
H11A H 0.8171 0.2050 0.7073 0.079 Uiso 1 1 calc R . .
H11B H 0.9318 0.1945 0.6527 0.079 Uiso 1 1 calc R . .
H11C H 0.8774 0.0482 0.6926 0.079 Uiso 1 1 calc R . .
C12 C 0.6611(3) 0.0454(3) 0.5947(3) 0.0322(7) Uani 1 1 d . . .
H12A H 0.6216 0.1036 0.6388 0.048 Uiso 1 1 calc R . .
H12B H 0.6822 -0.0519 0.6212 0.048 Uiso 1 1 calc R . .
H12C H 0.6066 0.0337 0.5372 0.048 Uiso 1 1 calc R . .
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'
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 Re O3 106.25(14) . . ?
O1 Re O2 106.17(13) . . ?
O3 Re O2 107.50(12) . . ?
O1 Re N2 98.54(11) . . ?
O3 Re N2 111.69(11) . . ?
O2 Re N2 124.78(10) . . ?
O1 Re N1 136.84(11) . . ?
O3 Re N1 100.07(11) . . ?
O2 Re N1 97.51(10) . . ?
N2 Re N1 39.15(9) . . ?
C1 N1 N2 108.7(2) . . ?
C1 N1 Re 160.3(2) . . ?
N2 N1 Re 67.22(14) . . ?
C3 N2 N1 109.4(2) . . ?
C3 N2 Re 159.2(2) . . ?
N1 N2 Re 73.62(14) . . ?
N1 C1 C2 107.8(2) . . ?
N1 C1 C4 120.6(2) . . ?
C2 C1 C4 131.4(3) . . ?
C3 C2 C1 106.8(2) . . ?
C3 C2 C8 127.1(3) . . ?
C1 C2 C8 126.1(3) . . ?
N2 C3 C2 107.1(2) . . ?
N2 C3 C9 121.0(2) . . ?
C2 C3 C9 131.9(3) . . ?
C1 C4 C5 109.4(2) . . ?
C1 C4 C6 110.8(2) . . ?
C5 C4 C6 108.7(3) . . ?
C1 C4 C7 108.4(2) . . ?
C5 C4 C7 108.8(3) . . ?
C6 C4 C7 110.7(3) . . ?
C3 C9 C11 110.3(3) . . ?
C3 C9 C12 111.2(2) . . ?
C11 C9 C12 108.5(3) . . ?
C3 C9 C10 107.8(3) . . ?
C11 C9 C10 109.3(3) . . ?
C12 C9 C10 109.7(3) . . ?
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 O1 1.699(3) . ?
Re O3 1.698(2) . ?
Re O2 1.705(2) . ?
Re N2 2.022(2) . ?
Re N1 2.104(2) . ?
N1 C1 1.334(4) . ?
N1 N2 1.385(3) . ?
N2 C3 1.354(4) . ?
C1 C2 1.421(4) . ?
C1 C4 1.516(4) . ?
C2 C3 1.399(4) . ?
C2 C8 1.502(4) . ?
C3 C9 1.511(4) . ?
C4 C5 1.533(4) . ?
C4 C6 1.533(4) . ?
C4 C7 1.537(4) . ?
C9 C11 1.522(5) . ?
C9 C12 1.539(4) . ?
C9 C10 1.548(5) . ?
