#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:25:54 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178715 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/26/4082605.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_4082605
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            'C51 H39 N12 O9 Re3'
_chemical_formula_weight         1522.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7152(3)
_cell_length_b                   19.7722(4)
_cell_length_c                   20.2242(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6284.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60854
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    5.820
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.530
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1472P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2349
_reflns_number_gt                3938
_reflns_number_total             7073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4005065_si_003.cif
_cod_data_source_block           i8198
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Pnma
_cod_database_code               4082605
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Re1 Re 0.72108(5) 0.2500 0.41977(4) 0.0623(3) Uani 1 2 d S
Re2 Re 0.81562(3) 0.08954(2) 0.68358(3) 0.0579(2) Uani 1 1 d .
O1 O 0.5526(11) 0.2500 0.4904(11) 0.151(7) Uani 1 2 d S
O2 O 0.6543(8) 0.1408(7) 0.3276(6) 0.116(4) Uani 1 1 d .
O3 O 0.6299(7) 0.1226(5) 0.7112(5) 0.090(3) Uani 1 1 d .
O4 O 0.8395(7) 0.0617(7) 0.8322(5) 0.098(3) Uani 1 1 d .
O5 O 0.7660(7) -0.0592(5) 0.6606(6) 0.106(4) Uani 1 1 d .
N1 N 0.9877(10) 0.2500 0.3650(7) 0.065(4) Uani 1 2 d S
N2 N 0.8486(9) 0.2500 0.3755(7) 0.060(3) Uani 1 2 d S
N3 N 1.0784(6) 0.0912(4) 0.6195(5) 0.058(2) Uani 1 1 d .
N4 N 0.9486(6) 0.0722(5) 0.6609(5) 0.061(3) Uani 1 1 d .
N5 N 0.7749(6) 0.1736(5) 0.4862(5) 0.065(3) Uani 1 1 d .
N6 N 0.8081(6) 0.1166(5) 0.5783(5) 0.060(3) Uani 1 1 d .
N7 N 0.8576(5) 0.1933(4) 0.7009(5) 0.053(2) Uani 1 1 d .
C1 C 1.0943(9) 0.2500 0.4548(8) 0.056(4) Uani 1 2 d S
C2 C 1.1031(7) 0.1882(6) 0.4874(6) 0.059(3) Uani 1 1 d .
C3 C 1.1279(7) 0.1872(5) 0.5512(7) 0.061(3) Uani 1 1 d .
C4 C 1.1373(10) 0.2500 0.5883(11) 0.080(6) Uani 1 2 d S
C5 C 0.9173(10) 0.2500 0.4074(8) 0.054(4) Uani 1 2 d S
H5 H 0.9209 0.2500 0.4533 0.065 Uiso 1 2 calc SR
C6 C 0.9553(12) 0.2500 0.2998(11) 0.072(5) Uani 1 2 d S
C7 C 0.9950(15) 0.2500 0.2384(9) 0.076(5) Uani 1 2 d S
H7 H 1.0540 0.2500 0.2344 0.092 Uiso 1 2 calc SR
C8 C 0.945(2) 0.2500 0.1860(11) 0.103(8) Uani 1 2 d S
H8 H 0.9702 0.2500 0.1444 0.123 Uiso 1 2 calc SR
C9 C 0.857(2) 0.2500 0.1898(13) 0.118(9) Uani 1 2 d S
H9 H 0.8245 0.2500 0.1511 0.142 Uiso 1 2 calc SR
C10 C 0.8149(13) 0.2500 0.2515(10) 0.078(5) Uani 1 2 d S
H10 H 0.7560 0.2500 0.2558 0.093 Uiso 1 2 calc SR
C11 C 0.8698(13) 0.2500 0.3055(8) 0.059(4) Uani 1 2 d S
C12 C 1.0796(11) 0.2500 0.3806(10) 0.079(6) Uani 1 2 d S
H12A H 1.1061 0.2897 0.3613 0.095 Uiso 0.50 1 calc PR
H12B H 1.1061 0.2103 0.3613 0.095 Uiso 0.50 1 calc PR
C13 C 0.9989(8) 0.1132(6) 0.6241(6) 0.062(3) Uani 1 1 d .
H13 H 0.9797 0.1527 0.6041 0.074 Uiso 1 1 calc R
C14 C 1.0830(7) 0.0310(5) 0.6576(6) 0.058(3) Uani 1 1 d .
C15 C 1.1507(9) -0.0117(6) 0.6677(7) 0.071(4) Uani 1 1 d .
H15 H 1.2033 -0.0042 0.6478 0.086 Uiso 1 1 calc R
C16 C 1.1367(11) -0.0669(7) 0.7093(8) 0.087(4) Uani 1 1 d .
H16 H 1.1807 -0.0971 0.7178 0.105 Uiso 1 1 calc R
C17 C 1.0580(12) -0.0770(7) 0.7377(8) 0.099(5) Uani 1 1 d .
H17 H 1.0519 -0.1129 0.7669 0.118 Uiso 1 1 calc R
C18 C 0.9835(10) -0.0345(6) 0.7247(7) 0.081(4) Uani 1 1 d .
H18 H 0.9296 -0.0427 0.7419 0.097 Uiso 1 1 calc R
C19 C 1.0039(8) 0.0220(5) 0.6815(5) 0.056(3) Uani 1 1 d .
C20 C 1.1507(7) 0.1233(6) 0.5869(6) 0.063(3) Uani 1 1 d .
H20A H 1.1752 0.0917 0.5556 0.076 Uiso 1 1 calc R
H20B H 1.1938 0.1334 0.6198 0.076 Uiso 1 1 calc R
C21 C 1.0872(9) 0.1208(7) 0.4525(8) 0.090(4) Uani 1 1 d .
H21A H 1.1383 0.1065 0.4305 0.135 Uiso 1 1 calc R
H21B H 1.0425 0.1262 0.4205 0.135 Uiso 1 1 calc R
H21C H 1.0708 0.0873 0.4844 0.135 Uiso 1 1 calc R
C22 C 1.1623(12) 0.2500 0.6613(10) 0.074(5) Uani 1 2 d S
H22A H 1.1601 0.2954 0.6781 0.111 Uiso 0.50 1 calc PR
H22B H 1.2190 0.2326 0.6659 0.111 Uiso 0.50 1 calc PR
H22C H 1.1234 0.2220 0.6857 0.111 Uiso 0.50 1 calc PR
C23 C 0.7628(7) 0.1664(6) 0.5510(6) 0.060(3) Uani 1 1 d .
H23 H 0.7260 0.1937 0.5752 0.072 Uiso 1 1 calc R
C24 C 0.8342(9) 0.1226(6) 0.4699(7) 0.079(4) Uani 1 1 d .
H24 H 0.8569 0.1140 0.4283 0.094 Uiso 1 1 calc R
C25 C 0.8524(9) 0.0878(6) 0.5276(6) 0.066(3) Uani 1 1 d .
H25 H 0.8887 0.0508 0.5312 0.080 Uiso 1 1 calc R
C26 C 0.8182(9) 0.2500 0.6874(7) 0.049(4) Uani 1 2 d S
H26 H 0.7641 0.2500 0.6687 0.059 Uiso 1 2 calc SR
C27 C 0.9284(8) 0.2148(6) 0.7270(7) 0.071(3) Uani 1 1 d .
H27 H 0.9719 0.1875 0.7431 0.085 Uiso 1 1 calc R
C28 C 0.6181(12) 0.2500 0.4634(11) 0.085(6) Uani 1 2 d S
C29 C 0.6777(8) 0.1805(8) 0.3611(8) 0.081(4) Uani 1 1 d .
C30 C 0.6996(8) 0.1097(7) 0.7008(7) 0.059(3) Uani 1 1 d .
C31 C 0.8288(9) 0.0713(7) 0.7733(8) 0.075(4) Uani 1 1 d .
C32 C 0.7828(8) -0.0048(7) 0.6665(6) 0.068(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'
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
C28 Re1 C29 89.1(7) . .
C28 Re1 C29 89.1(7) . 7_565
C29 Re1 C29 90.2(8) . 7_565
C28 Re1 N5 92.6(6) . 7_565
C29 Re1 N5 177.8(5) . 7_565
C29 Re1 N5 91.3(5) 7_565 7_565
C28 Re1 N5 92.6(6) . .
C29 Re1 N5 91.3(5) . .
C29 Re1 N5 177.8(5) 7_565 .
N5 Re1 N5 87.2(5) 7_565 .
C28 Re1 N2 175.5(8) . .
C29 Re1 N2 94.1(5) . .
C29 Re1 N2 94.1(5) 7_565 .
N5 Re1 N2 84.1(4) 7_565 .
N5 Re1 N2 84.1(4) . .
C31 Re2 C30 88.2(6) . .
C31 Re2 C32 90.9(6) . .
C30 Re2 C32 88.8(5) . .
C31 Re2 N4 93.9(5) . .
C30 Re2 N4 176.6(4) . .
C32 Re2 N4 93.7(4) . .
C31 Re2 N7 89.5(5) . .
C30 Re2 N7 93.6(5) . .
C32 Re2 N7 177.5(4) . .
N4 Re2 N7 83.8(3) . .
C31 Re2 N6 175.6(5) . .
C30 Re2 N6 94.3(5) . .
C32 Re2 N6 92.7(4) . .
N4 Re2 N6 83.4(4) . .
N7 Re2 N6 86.7(4) . .
C5 N1 C6 106.7(15) . .
C5 N1 C12 129.9(14) . .
C6 N1 C12 123.4(15) . .
C5 N2 C11 107.5(15) . .
C5 N2 Re1 125.1(12) . .
C11 N2 Re1 127.3(12) . .
C13 N3 C14 106.6(10) . .
C13 N3 C20 128.5(10) . .
C14 N3 C20 124.8(9) . .
C13 N4 C19 103.1(10) . .
C13 N4 Re2 125.8(7) . .
C19 N4 Re2 131.0(8) . .
C23 N5 C24 104.2(10) . .
C23 N5 Re1 128.5(8) . .
C24 N5 Re1 127.2(9) . .
C23 N6 C25 105.6(11) . .
C23 N6 Re2 127.5(8) . .
C25 N6 Re2 126.8(9) . .
C27 N7 C26 102.1(10) . .
C27 N7 Re2 129.1(8) . .
C26 N7 Re2 128.9(8) . .
C2 C1 C2 122.2(15) 7_565 .
C2 C1 C12 118.9(8) 7_565 .
C2 C1 C12 118.9(8) . .
C3 C2 C1 119.6(11) . .
C3 C2 C21 118.5(12) . .
C1 C2 C21 121.8(12) . .
C2 C3 C4 120.6(13) . .
C2 C3 C20 122.8(11) . .
C4 C3 C20 116.5(13) . .
C3 C4 C3 116.8(19) . 7_565
C3 C4 C22 121.5(9) . .
C3 C4 C22 121.5(9) 7_565 .
N2 C5 N1 111.4(15) . .
C11 C6 C7 122(2) . .
C11 C6 N1 106.2(16) . .
C7 C6 N1 132.3(19) . .
C8 C7 C6 117(2) . .
C7 C8 C9 123(2) . .
C8 C9 C10 121(2) . .
C11 C10 C9 114(2) . .
C6 C11 C10 123.4(17) . .
C6 C11 N2 108.2(16) . .
C10 C11 N2 128.4(17) . .
N1 C12 C1 111.0(14) . .
N3 C13 N4 113.1(10) . .
C19 C14 C15 125.4(12) . .
C19 C14 N3 105.1(10) . .
C15 C14 N3 129.5(12) . .
C14 C15 C16 116.6(13) . .
C17 C16 C15 120.4(14) . .
C16 C17 C18 124.1(15) . .
C19 C18 C17 111.8(14) . .
C14 C19 N4 112.1(10) . .
C14 C19 C18 121.5(11) . .
N4 C19 C18 126.3(12) . .
N3 C20 C3 113.5(9) . .
N5 C23 N6 114.2(11) . .
C25 C24 N5 107.2(11) . .
N6 C25 C24 108.7(11) . .
N7 C26 N7 117.7(13) 7_565 .
N7 C26 C27 38.8(6) 7_565 7_565
N7 C26 C27 78.9(9) . 7_565
N7 C26 C27 78.9(9) 7_565 .
N7 C26 C27 38.8(6) . .
C27 C26 C27 40.1(7) 7_565 .
N7 C27 C27 109.1(7) . 7_565
N7 C27 C26 39.1(6) . .
C27 C27 C26 70.0(4) 7_565 .
O1 C28 Re1 179(2) . .
O2 C29 Re1 178.9(14) . .
O3 C30 Re2 179.2(13) . .
O4 C31 Re2 177.3(13) . .
O5 C32 Re2 175.7(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C28 1.84(2) .
Re1 C29 1.939(16) .
Re1 C29 1.939(16) 7_565
Re1 N5 2.190(10) 7_565
Re1 N5 2.190(9) .
Re1 N2 2.194(15) .
Re2 C31 1.863(17) .
Re2 C30 1.898(12) .
Re2 C32 1.966(15) .
Re2 N4 2.166(10) .
Re2 N7 2.183(9) .
Re2 N6 2.198(10) .
O1 C28 1.17(2) .
O2 C29 1.100(16) .
O3 C30 1.146(13) .
O4 C31 1.217(17) .
O5 C32 1.114(15) .
N1 C5 1.399(19) .
N1 C6 1.41(2) .
N1 C12 1.48(2) .
N2 C5 1.26(2) .
N2 C11 1.46(2) .
N3 C13 1.326(14) .
N3 C14 1.419(14) .
N3 C20 1.459(14) .
N4 C13 1.356(14) .
N4 C19 1.385(14) .
N5 C23 1.333(15) .
N5 C24 1.413(15) .
N6 C23 1.334(14) .
N6 C25 1.365(16) .
N7 C27 1.303(15) .
N7 C26 1.310(11) .
C1 C2 1.396(14) 7_565
C1 C2 1.396(14) .
C1 C12 1.52(3) .
C2 C3 1.348(17) .
C2 C21 1.529(16) .
C3 C4 1.457(16) .
C3 C20 1.499(16) .
C4 C3 1.457(16) 7_565
C4 C22 1.53(3) .
C6 C11 1.35(3) .
C6 C7 1.39(3) .
C7 C8 1.32(3) .
C8 C9 1.39(4) .
C9 C10 1.41(3) .
C10 C11 1.39(3) .
C14 C19 1.346(16) .
C14 C15 1.374(16) .
C15 C16 1.396(19) .
C16 C17 1.38(2) .
C17 C18 1.46(2) .
C18 C19 1.454(16) .
C24 C25 1.385(18) .
C26 N7 1.310(11) 7_565
C26 C27 2.032(19) 7_565
C26 C27 2.032(19) .
C27 C27 1.39(2) 7_565
