#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:25:54 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178715 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/26/4082606.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_4082606
loop_
_publ_author_name
'Lin, Shih-Ming'
'Velayudham, Murugesan'
'Tsai, Chi-Hwe'
'Chang, Che-Hao'
'Lee, Chung-Chou'
'Luo, Tzuoo-Tsair'
'Thanasekaran, Pounraj'
'Lu, Kuang-Lieh'
_publ_section_title
;
 A Molecular Triangle as a Precursor Toward the Assembly of a Jar-Shaped
 Metallasupramolecule
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              40
_journal_paper_doi               10.1021/om4005065
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C21 H9 N6 O12 Re3'
_chemical_formula_weight         1095.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 106.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0210(14)
_cell_length_b                   19.501(4)
_cell_length_c                   10.380(2)
_cell_measurement_reflns_used    5181
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.24
_cell_measurement_theta_min      3.67
_cell_volume                     1365.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2475
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    13.337
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0151
_refine_ls_R_factor_gt           0.0128
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0174P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0313
_refine_ls_wR_factor_ref         0.0316
_reflns_number_gt                2299
_reflns_number_total             2475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4005065_si_002.cif
_cod_data_source_block           i6548
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4082606
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.103129(17) 0.089405(5) 0.279283(12) 0.01407(5) Uani 1 1 d .
Re2 Re -0.10039(2) 0.2500 0.755652(17) 0.01559(5) Uani 1 2 d S
O6 O 0.1423(3) 0.06175(11) -0.0046(2) 0.0291(5) Uani 1 1 d .
O7 O 0.2726(3) -0.05250(10) 0.3804(2) 0.0270(5) Uani 1 1 d .
O8 O 0.5394(3) 0.14072(11) 0.3449(2) 0.0284(5) Uani 1 1 d .
O9 O -0.3321(3) 0.03099(10) 0.1852(2) 0.0294(5) Uani 1 1 d .
O10 O -0.2826(3) 0.13488(10) 0.8875(2) 0.0287(5) Uani 1 1 d .
O11 O -0.5131(4) 0.2500 0.5406(3) 0.0289(7) Uani 1 2 d S
O12 O 0.2760(5) 0.2500 1.0035(3) 0.0382(8) Uani 1 2 d S
N1 N 0.0964(3) 0.11821(11) 0.4808(2) 0.0143(5) Uani 1 1 d .
N2 N 0.0333(3) 0.17592(11) 0.6504(2) 0.0156(5) Uani 1 1 d .
N3 N -0.0082(3) 0.19266(11) 0.2289(2) 0.0138(5) Uani 1 1 d .
C1 C -0.0157(4) 0.16486(12) 0.5182(3) 0.0163(6) Uani 1 1 d .
H1 H -0.1189 0.1877 0.4579 0.020 Uiso 1 1 calc R
C2 C 0.1884(4) 0.13205(15) 0.7015(3) 0.0227(7) Uani 1 1 d .
H2 H 0.2555 0.1270 0.7918 0.027 Uiso 1 1 calc R
C3 C 0.2275(5) 0.09742(15) 0.5994(3) 0.0224(7) Uani 1 1 d .
H3 H 0.3268 0.0648 0.6076 0.027 Uiso 1 1 calc R
C4 C 0.0968(6) 0.2500 0.2642(4) 0.0157(9) Uani 1 2 d S
H4 H 0.2311 0.2500 0.3095 0.019 Uiso 1 2 calc SR
C5 C -0.1967(4) 0.21533(13) 0.1658(3) 0.0168(6) Uani 1 1 d .
H5 H -0.3060 0.1875 0.1292 0.020 Uiso 1 1 calc R
C6 C 0.1246(5) 0.07121(14) 0.1008(3) 0.0208(7) Uani 1 1 d .
C7 C 0.2056(4) -0.00067(15) 0.3410(3) 0.0188(6) Uani 1 1 d .
C8 C 0.3803(5) 0.12312(14) 0.3242(3) 0.0184(6) Uani 1 1 d .
C9 C -0.1768(5) 0.05284(14) 0.2239(3) 0.0189(7) Uani 1 1 d .
C10 C -0.2135(4) 0.17783(15) 0.8409(3) 0.0211(7) Uani 1 1 d .
C11 C -0.3559(6) 0.2500 0.6130(4) 0.0200(9) Uani 1 2 d S
C12 C 0.1441(6) 0.2500 0.9113(4) 0.0242(10) Uani 1 2 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'
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
C6 Re1 C7 91.73(12) . .
C6 Re1 C8 87.35(12) . .
C7 Re1 C8 88.45(11) . .
C6 Re1 C9 89.48(12) . .
C7 Re1 C9 90.96(11) . .
C8 Re1 C9 176.76(11) . .
C6 Re1 N3 93.32(10) . .
C7 Re1 N3 174.85(10) . .
C8 Re1 N3 90.76(10) . .
C9 Re1 N3 90.12(10) . .
C6 Re1 N1 174.67(10) . .
C7 Re1 N1 91.20(10) . .
C8 Re1 N1 88.27(10) . .
C9 Re1 N1 94.93(10) . .
N3 Re1 N1 83.69(8) . .
C10 Re2 C10 92.68(17) 4_565 .
C10 Re2 C11 86.60(12) 4_565 .
C10 Re2 C11 86.60(12) . .
C10 Re2 C12 89.99(12) 4_565 .
C10 Re2 C12 89.99(12) . .
C11 Re2 C12 175.07(17) . .
C10 Re2 N2 175.24(10) 4_565 .
C10 Re2 N2 92.04(10) . .
C11 Re2 N2 92.98(10) . .
C12 Re2 N2 90.71(11) . .
C10 Re2 N2 92.04(10) 4_565 4_565
C10 Re2 N2 175.24(10) . 4_565
C11 Re2 N2 92.98(10) . 4_565
C12 Re2 N2 90.71(11) . 4_565
N2 Re2 N2 83.24(12) . 4_565
C1 N1 C3 104.1(2) . .
C1 N1 Re1 128.99(19) . .
C3 N1 Re1 126.52(18) . .
C1 N2 C2 104.3(2) . .
C1 N2 Re2 126.79(19) . .
C2 N2 Re2 128.85(19) . .
C4 N3 C5 104.3(2) . .
C4 N3 Re1 125.2(2) . .
C5 N3 Re1 130.31(17) . .
N1 C1 N2 113.9(2) . .
C3 C2 N2 108.8(3) . .
C2 C3 N1 108.9(3) . .
N3 C4 N3 114.0(3) . 4_565
C5 C5 N3 108.73(14) 4_565 .
O6 C6 Re1 177.9(3) . .
O7 C7 Re1 177.3(3) . .
O8 C8 Re1 176.9(3) . .
O9 C9 Re1 175.6(3) . .
O10 C10 Re2 178.1(3) . .
O11 C11 Re2 173.1(3) . .
O12 C12 Re2 176.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C6 1.933(3) .
Re1 C7 1.938(3) .
Re1 C8 1.983(3) .
Re1 C9 2.019(3) .
Re1 N3 2.171(2) .
Re1 N1 2.179(2) .
Re2 C10 1.946(3) 4_565
Re2 C10 1.946(3) .
Re2 C11 1.984(5) .
Re2 C12 2.004(5) .
Re2 N2 2.175(2) .
Re2 N2 2.175(2) 4_565
O6 C6 1.149(4) .
O7 C7 1.142(3) .
O8 C8 1.131(3) .
O9 C9 1.135(3) .
O10 C10 1.140(3) .
O11 C11 1.150(5) .
O12 C12 1.133(5) .
N1 C1 1.330(3) .
N1 C3 1.378(4) .
N2 C1 1.336(3) .
N2 C2 1.370(3) .
N3 C4 1.334(3) .
N3 C5 1.377(3) .
C2 C3 1.348(4) .
C4 N3 1.334(3) 4_565
C5 C5 1.352(5) 4_565
