#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/82/7008297.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_7008297
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            'C11 H21 N2 O4 Re'
_chemical_formula_weight         431.50
_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                 103.657(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7531(4)
_cell_length_b                   10.1836(5)
_cell_length_c                   15.4082(6)
_cell_measurement_temperature    133(2)
_cell_volume                     1487.10(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30138
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    8.179
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0139
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0104P)²+2.5068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0321
_reflns_number_gt                2486
_reflns_number_total             2548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b501025j.txt
_cod_data_source_block           g42
_cod_database_code               7008297
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 0.172851(10) 0.354598(10) 0.535720(7) 0.01846(5) Uani 1 1 d . . .
N1 N 0.0199(2) 0.4111(2) 0.74752(15) 0.0209(5) Uani 1 1 d . . .
N2 N -0.1177(2) 0.4314(2) 0.70715(15) 0.0208(5) Uani 1 1 d . . .
O1 O 0.2086(2) 0.42092(19) 0.64249(12) 0.0235(4) Uani 1 1 d . . .
O2 O 0.3220(2) 0.2788(2) 0.52004(14) 0.0329(5) Uani 1 1 d . . .
O3 O 0.0415(2) 0.2408(2) 0.52567(16) 0.0400(6) Uani 1 1 d . . .
O4 O 0.1247(2) 0.4769(2) 0.45580(14) 0.0379(5) Uani 1 1 d . . .
C5 C 0.1740(3) 0.3454(3) 0.89266(18) 0.0198(6) Uani 1 1 d . . .
C6 C -0.1959(3) 0.4108(3) 0.76656(17) 0.0188(5) Uani 1 1 d . . .
C7 C 0.0312(3) 0.3755(2) 0.83233(17) 0.0179(5) Uani 1 1 d . . .
C8 C -0.1040(3) 0.3751(3) 0.84639(18) 0.0194(5) Uani 1 1 d . . .
H8A H -0.1292 0.3542 0.9007 0.023 Uiso 1 1 calc R . .
C9 C 0.2482(3) 0.2414(3) 0.8480(2) 0.0305(7) Uani 1 1 d . . .
H9A H 0.1893 0.1625 0.8360 0.046 Uiso 1 1 calc R . .
H9B H 0.3394 0.2192 0.8877 0.046 Uiso 1 1 calc R . .
H9C H 0.2632 0.2762 0.7916 0.046 Uiso 1 1 calc R . .
C10 C -0.3549(3) 0.4233(3) 0.74161(18) 0.0234(6) Uani 1 1 d . . .
C11 C 0.1543(3) 0.2930(3) 0.9820(2) 0.0334(7) Uani 1 1 d . . .
H11A H 0.1092 0.3604 1.0112 0.050 Uiso 1 1 calc R . .
H11B H 0.2465 0.2705 1.0205 0.050 Uiso 1 1 calc R . .
H11C H 0.0947 0.2144 0.9716 0.050 Uiso 1 1 calc R . .
C12 C -0.4184(3) 0.2849(3) 0.7391(3) 0.0414(8) Uani 1 1 d . . .
H12A H -0.3848 0.2310 0.6957 0.062 Uiso 1 1 calc R . .
H12B H -0.5215 0.2906 0.7218 0.062 Uiso 1 1 calc R . .
H12C H -0.3892 0.2447 0.7984 0.062 Uiso 1 1 calc R . .
C13 C -0.4053(3) 0.4873(3) 0.65000(19) 0.0264(6) Uani 1 1 d . . .
H13A H -0.3646 0.5755 0.6512 0.040 Uiso 1 1 calc R . .
H13B H -0.5085 0.4936 0.6351 0.040 Uiso 1 1 calc R . .
H13C H -0.3751 0.4340 0.6049 0.040 Uiso 1 1 calc R . .
C14 C 0.2613(3) 0.4717(3) 0.9084(2) 0.0327(7) Uani 1 1 d . . .
H14A H 0.2136 0.5366 0.9379 0.049 Uiso 1 1 calc R . .
H14B H 0.2715 0.5066 0.8510 0.049 Uiso 1 1 calc R . .
H14C H 0.3548 0.4526 0.9465 0.049 Uiso 1 1 calc R . .
C15 C -0.4008(3) 0.5070(4) 0.8123(2) 0.0445(9) Uani 1 1 d . . .
H15A H -0.3566 0.5938 0.8150 0.067 Uiso 1 1 calc R . .
H15B H -0.3715 0.4640 0.8706 0.067 Uiso 1 1 calc R . .
H15C H -0.5037 0.5167 0.7965 0.067 Uiso 1 1 calc R . .
H1 H 0.077(3) 0.418(3) 0.718(2) 0.024(8) Uiso 1 1 d . . .
H2 H -0.138(3) 0.461(3) 0.654(2) 0.022(8) Uiso 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'
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
O3 Re1 O2 108.97(11) . . ?
O3 Re1 O1 109.18(11) . . ?
O2 Re1 O1 108.76(9) . . ?
O3 Re1 O4 110.56(11) . . ?
O2 Re1 O4 108.64(11) . . ?
O1 Re1 O4 110.68(10) . . ?
C7 N1 N2 109.6(2) . . ?
C6 N2 N1 108.9(2) . . ?
C7 C5 C14 109.0(2) . . ?
C7 C5 C11 109.3(2) . . ?
C14 C5 C11 109.5(2) . . ?
C7 C5 C9 109.1(2) . . ?
C14 C5 C9 110.3(2) . . ?
C11 C5 C9 109.6(2) . . ?
N2 C6 C8 107.1(2) . . ?
N2 C6 C10 121.9(2) . . ?
C8 C6 C10 131.0(2) . . ?
N1 C7 C8 107.0(2) . . ?
N1 C7 C5 120.5(2) . . ?
C8 C7 C5 132.5(2) . . ?
C7 C8 C6 107.4(2) . . ?
C6 C10 C13 111.0(2) . . ?
C6 C10 C15 108.7(2) . . ?
C13 C10 C15 109.6(3) . . ?
C6 C10 C12 108.2(2) . . ?
C13 C10 C12 109.2(2) . . ?
C15 C10 C12 110.2(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
Re1 O3 1.708(2) . ?
Re1 O2 1.714(2) . ?
Re1 O1 1.7359(18) . ?
Re1 O4 1.736(2) . ?
N1 C7 1.335(3) . ?
N1 N2 1.355(3) . ?
N2 C6 1.339(3) . ?
C5 C7 1.512(4) . ?
C5 C14 1.530(4) . ?
C5 C11 1.530(4) . ?
C5 C9 1.534(4) . ?
C6 C8 1.389(4) . ?
C6 C10 1.513(4) . ?
C7 C8 1.386(4) . ?
C10 C13 1.527(4) . ?
C10 C15 1.530(4) . ?
C10 C12 1.537(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O1 0.81(3) 1.92(3) 2.725(3) 175(3) .
N2 H2 O4 0.85(3) 1.84(3) 2.665(3) 163(3) 3_566
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652708
