#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:19:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179241 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/61/4316151.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_4316151
loop_
_publ_author_name
'Yi-Hsiu Tseng'
'Dibyendu Bhattacharya'
'Shih-Ming Lin'
'P. Thanasekaran'
'Jing-Yun Wu'
'Li-Wei Lee'
'M. Sathiyendiran'
'Mei-Lin Ho'
'Min-Wen Chung'
'Kung-Chung Hsu'
'Pi-Tai Chou'
'Kuang-Lieh Lu'
_publ_section_title
;
 Highly Emissive Cyclometalated Rhenium Metallacycles:
 Structure-Luminescence Relationship
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6805
_journal_page_last               6807
_journal_paper_doi               10.1021/ic100882u
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C50 H39 N7 O7 Re2'
_chemical_formula_sum            'C50 H39 N7 O7 Re2'
_chemical_formula_weight         1222.28
_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                   11.0604(3)
_cell_length_b                   15.2102(4)
_cell_length_c                   27.2689(8)
_cell_measurement_reflns_used    14619
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     4587.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski&Minor 1997)'
_computing_molecular_graphics    'WinGX publication routines (Farrugia, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1106
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12395
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    5.333
_exptl_absorpt_correction_T_max  0.9008
_exptl_absorpt_correction_T_min  0.2242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.242
_refine_diff_density_min         -2.571
_refine_diff_density_rms         0.494
_refine_ls_extinction_coef       0.0064(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0866
_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)+(0.1281P)²+50.4158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2289
_refine_ls_wR_factor_ref         0.2570
_reflns_number_gt                3084
_reflns_number_total             4185
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic100882u_si_001_1.cif
_cod_data_source_block           cpd1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4316151
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.20517(5) 0.06071(4) 0.11772(2) 0.0378(4) Uani 1 1 d U . .
O1 O 0.0936(16) -0.0760(10) 0.0461(6) 0.092(5) Uani 1 1 d U . .
O2 O 0.0070(13) 0.0057(10) 0.1890(6) 0.083(5) Uani 1 1 d U . .
O3 O 0.3801(14) -0.0704(8) 0.1645(6) 0.079(5) Uani 1 1 d U . .
O4 O 0.2305(17) 0.7500 0.0706(7) 0.076(6) Uani 1 2 d S . .
N1 N 0.3440(11) 0.1015(8) 0.0641(4) 0.035(2) Uani 1 1 d U . .
N2 N 0.5276(11) 0.1363(10) 0.0373(5) 0.044(3) Uani 1 1 d . . .
N3 N 0.2758(10) 0.1758(8) 0.1567(4) 0.034(2) Uani 1 1 d U . .
N4 N 0.0998(10) 0.1670(8) 0.0862(5) 0.031(2) Uani 0.50 1 d PU . 1
C20 C 0.0998(10) 0.1670(8) 0.0862(5) 0.031(2) Uani 0.50 1 d PU . 2
C1 C 0.1374(16) -0.0208(10) 0.0738(6) 0.044(2) Uani 1 1 d U . .
C2 C 0.0817(15) 0.0265(11) 0.1631(6) 0.048(4) Uani 1 1 d U . .
C3 C 0.3133(15) -0.0217(10) 0.1482(7) 0.044(2) Uani 1 1 d U . .
C4 C 0.3422(15) 0.1060(11) 0.0135(6) 0.043(4) Uani 1 1 d U . .
C5 C 0.2452(17) 0.0922(14) -0.0207(6) 0.055(4) Uani 1 1 d U . .
H5 H 0.1659 0.0784 -0.0097 0.066 Uiso 1 1 calc R . .
C6 C 0.271(2) 0.0995(18) -0.0692(7) 0.077(6) Uani 1 1 d U . .
H6 H 0.2071 0.0941 -0.0924 0.092 Uiso 1 1 calc R . .
C7 C 0.3865(19) 0.1146(19) -0.0859(7) 0.084(6) Uani 1 1 d U . .
H7 H 0.4016 0.1132 -0.1202 0.101 Uiso 1 1 calc R . .
C8 C 0.4844(18) 0.1323(15) -0.0532(6) 0.064(5) Uani 1 1 d U . .
H8 H 0.5626 0.1482 -0.0646 0.077 Uiso 1 1 calc R . .
C9 C 0.4582(16) 0.1248(13) -0.0042(6) 0.055(5) Uani 1 1 d U . .
C10 C 0.4581(14) 0.1208(11) 0.0752(6) 0.043(4) Uani 1 1 d . . .
H10 H 0.4869 0.1231 0.1080 0.052 Uiso 1 1 calc R . .
C11 C 0.6592(14) 0.1507(12) 0.0365(7) 0.048(4) Uani 1 1 d U . .
H11A H 0.6817 0.1819 0.0060 0.057 Uiso 1 1 calc R . .
H11B H 0.7012 0.0932 0.0367 0.057 Uiso 1 1 calc R . .
C12 C 0.7001(12) 0.2047(14) 0.0807(6) 0.053(4) Uani 1 1 d U . .
C13 C 0.7411(17) 0.158(2) 0.1214(7) 0.079(6) Uani 1 1 d U . .
H13 H 0.7392 0.0955 0.1223 0.095 Uiso 1 1 calc R . .
C14 C 0.7856(16) 0.2077(18) 0.1615(8) 0.093(4) Uani 1 1 d U . .
H14 H 0.8165 0.1775 0.1893 0.112 Uiso 1 1 calc R . .
C15 C 0.5301(14) 0.2041(13) 0.2442(5) 0.050(4) Uani 1 1 d U . .
H15 H 0.5891 0.1738 0.2631 0.060 Uiso 1 1 calc R . .
C16 C 0.4469(13) 0.1563(11) 0.2176(6) 0.040(3) Uani 1 1 d U . .
H16 H 0.4450 0.0939 0.2182 0.048 Uiso 1 1 calc R . .
C17 C 0.3664(12) 0.2053(10) 0.1901(5) 0.034(3) Uani 1 1 d U . .
C18 C 0.2266(19) 0.2500 0.1410(8) 0.035(4) Uani 1 2 d SU . .
C19 C 0.1372(18) 0.2500 0.1029(7) 0.037(5) Uani 1 2 d SU . .
C21 C 0.0076(13) 0.1715(15) 0.0504(5) 0.051(4) Uani 1 1 d U . .
H21 H -0.0256 0.1186 0.0377 0.061 Uiso 1 1 calc R . 1
C22 C -0.0345(18) 0.2500 0.0337(8) 0.052(6) Uani 1 2 d SU . .
H22 H -0.0960 0.2500 0.0093 0.062 Uiso 1 2 calc SR . .
C23 C 0.224(3) 0.7500 0.1562(12) 0.089(7) Uani 1 2 d SU . .
H23A H 0.3122 0.7500 0.1530 0.133 Uiso 1 2 calc SR . .
H23B H 0.1983 0.6974 0.1741 0.133 Uiso 0.50 1 calc PR . .
H23C H 0.1983 0.8026 0.1741 0.133 Uiso 0.50 1 calc PR . .
C24 C 0.169(4) 0.7500 0.1076(12) 0.090(10) Uani 1 2 d SU . .
C25 C 0.038(3) 0.7500 0.1061(11) 0.089(7) Uani 1 2 d SU . .
H25A H 0.0104 0.7500 0.0719 0.133 Uiso 1 2 calc SR . .
H25B H 0.0068 0.8026 0.1227 0.133 Uiso 0.50 1 calc PR . .
H25C H 0.0068 0.6974 0.1227 0.133 Uiso 0.50 1 calc PR . .
C26 C 0.205(2) 0.658(3) 0.2850(8) 0.105(9) Uani 1 1 d U . .
H26 H 0.2053 0.5951 0.2849 0.05(16) Uiso 0.50 1 calc PR A 1
C29 C 0.203(5) 0.561(6) 0.2820(19) 0.119(16) Uani 0.50 1 d PU B 2
H29A H 0.1191 0.5410 0.2776 0.179 Uiso 0.50 1 calc PR B 2
H29B H 0.2354 0.5362 0.3124 0.179 Uiso 0.50 1 calc PR B 2
H29C H 0.2517 0.5417 0.2542 0.179 Uiso 0.50 1 calc PR B 2
C27 C 0.312(2) 0.706(2) 0.2899(8) 0.114(10) Uani 1 1 d U . .
H27 H 0.3862 0.6759 0.2934 0.137 Uiso 1 1 calc R . .
C28 C 0.093(2) 0.707(2) 0.2799(8) 0.113(10) Uani 1 1 d U . .
H28 H 0.0191 0.6765 0.2765 0.136 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'
Re Re -1.0185 7.2310 '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'
N N 0.0061 0.0033 '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
C1 Re1 C2 87.0(7) . . ?
C1 Re1 C3 95.4(7) . . ?
C2 Re1 C3 89.3(8) . . ?
C1 Re1 N4 91.4(6) . . ?
C2 Re1 N4 94.3(6) . . ?
C3 Re1 N4 172.5(6) . . ?
C1 Re1 N3 167.9(6) . . ?
C2 Re1 N3 99.1(6) . . ?
C3 Re1 N3 95.1(6) . . ?
N4 Re1 N3 77.8(4) . . ?
C1 Re1 N1 92.3(6) . . ?
C2 Re1 N1 178.5(7) . . ?
C3 Re1 N1 92.1(6) . . ?
N4 Re1 N1 84.4(4) . . ?
N3 Re1 N1 81.3(4) . . ?
C10 N1 C4 103.3(13) . . ?
C10 N1 Re1 124.9(10) . . ?
C4 N1 Re1 131.6(11) . . ?
C10 N2 C9 107.4(13) . . ?
C10 N2 C11 128.3(15) . . ?
C9 N2 C11 123.8(13) . . ?
C18 N3 C17 103.1(13) . . ?
C18 N3 Re1 112.2(10) . . ?
C17 N3 Re1 144.2(10) . . ?
C19 N4 C21 113.2(15) . . ?
C19 N4 Re1 112.5(10) . . ?
C21 N4 Re1 134.2(12) . . ?
O1 C1 Re1 178.1(16) . . ?
O2 C2 Re1 178.4(17) . . ?
O3 C3 Re1 177.2(16) . . ?
N1 C4 C9 109.9(15) . . ?
N1 C4 C5 130.7(16) . . ?
C9 C4 C5 119.5(16) . . ?
C6 C5 C4 117.6(19) . . ?
C6 C5 H5 121.2 . . ?
C4 C5 H5 121.2 . . ?
C5 C6 C7 122(2) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C6 C7 C8 122.0(19) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C9 C8 C7 115.6(19) . . ?
C9 C8 H8 122.2 . . ?
C7 C8 H8 122.2 . . ?
C8 C9 N2 132.2(18) . . ?
C8 C9 C4 123.0(18) . . ?
N2 C9 C4 104.7(13) . . ?
N2 C10 N1 114.7(14) . . ?
N2 C10 H10 122.6 . . ?
N1 C10 H10 122.6 . . ?
N2 C11 C12 111.2(13) . . ?
N2 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
N2 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C12 C12 C13 120.7(16) 8_565 . ?
C12 C12 C11 122.5(10) 8_565 . ?
C13 C12 C11 117(2) . . ?
C12 C13 C14 117(3) . . ?
C12 C13 H13 121.5 . . ?
C14 C13 H13 121.5 . . ?
C14 C14 C13 122.3(15) 8_565 . ?
C14 C14 H14 118.9 8_565 . ?
C13 C14 H14 118.9 . . ?
C16 C15 C15 121.8(10) . 8_565 ?
C16 C15 H15 119.1 . . ?
C15 C15 H15 119.1 8_565 . ?
C15 C16 C17 115.5(16) . . ?
C15 C16 H16 122.2 . . ?
C17 C16 H16 122.2 . . ?
C17 C17 C16 122.6(10) 8_565 . ?
C17 C17 N3 108.3(8) 8_565 . ?
C16 C17 N3 129.0(14) . . ?
N3 C18 N3 116.9(18) 8_565 . ?
N3 C18 C19 121.2(9) 8_565 . ?
N3 C18 C19 121.2(9) . . ?
C20 C19 N4 0.0(13) 8_565 8_565 ?
C20 C19 N4 127.9(18) 8_565 . ?
N4 C19 N4 127.9(18) 8_565 . ?
C20 C19 C18 116.0(9) 8_565 . ?
N4 C19 C18 116.0(9) 8_565 . ?
N4 C19 C18 116.0(9) . . ?
C22 C21 N4 121.4(18) . . ?
C22 C21 H21 119.3 . . ?
N4 C21 H21 119.3 . . ?
C21 C22 C21 123(2) . 8_565 ?
C21 C22 H22 118.6 . . ?
C21 C22 H22 118.6 8_565 . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O4 C24 C23 121(4) . . ?
O4 C24 C25 122(4) . . ?
C23 C24 C25 116(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C28 117(4) . . ?
C27 C26 C29 123(4) . . ?
C28 C26 C29 120(4) . . ?
C27 C26 H26 121.6 . . ?
C28 C26 H26 121.6 . . ?
C29 C26 H26 3.3 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C27 C26 122(2) 8_575 . ?
C27 C27 H27 119.0 8_575 . ?
C26 C27 H27 119.0 . . ?
C28 C28 C26 121(2) 8_575 . ?
C28 C28 H28 119.4 8_575 . ?
C26 C28 H28 119.4 . . ?
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 C1 1.879(16) . ?
Re1 C2 1.915(16) . ?
Re1 C3 1.922(18) . ?
Re1 N4 2.171(13) . ?
Re1 N3 2.192(12) . ?
Re1 N1 2.209(12) . ?
O1 C1 1.23(2) . ?
O2 C2 1.133(19) . ?
O3 C3 1.14(2) . ?
O4 C24 1.22(3) . ?
N1 C10 1.330(19) . ?
N1 C4 1.383(19) . ?
N2 C10 1.307(19) . ?
N2 C9 1.38(2) . ?
N2 C11 1.473(19) . ?
N3 C18 1.324(16) . ?
N3 C17 1.426(18) . ?
N4 C19 1.405(15) . ?
N4 C21 1.413(19) . ?
C4 C9 1.40(2) . ?
C4 C5 1.44(2) . ?
C5 C6 1.36(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.38(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.43(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.37(2) . ?
C8 H8 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.53(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.38(4) 8_565 ?
C12 C13 1.39(3) . ?
C13 C14 1.42(3) . ?
C13 H13 0.9500 . ?
C14 C14 1.29(6) 8_565 ?
C14 H14 0.9500 . ?
C15 C16 1.38(2) . ?
C15 C15 1.40(4) 8_565 ?
C15 H15 0.9500 . ?
C16 C17 1.38(2) . ?
C16 H16 0.9500 . ?
C17 C17 1.36(3) 8_565 ?
C18 N3 1.324(16) 8_565 ?
C18 C19 1.43(3) . ?
C19 C20 1.405(15) 8_565 ?
C19 N4 1.405(15) 8_565 ?
C21 C22 1.36(2) . ?
C21 H21 0.9500 . ?
C22 C21 1.36(2) 8_565 ?
C22 H22 0.9500 . ?
C23 C24 1.46(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.45(5) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.40(4) . ?
C26 C28 1.45(3) . ?
C26 C29 1.47(9) . ?
C26 H26 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C27 C27 1.33(7) 8_575 ?
C27 H27 0.9500 . ?
C28 C28 1.30(6) 8_575 ?
C28 H28 0.9500 . ?
