#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/30/7053053.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_7053053
loop_
_publ_author_name
'Chung, Wai-Kin'
'Wong, Keith Man-Chung'
'Lam, Wai Han'
'Zhu, Xiuling'
'Zhu, Nianyong'
'Kwok, Hoi-Sing'
'Yam, Vivian Wing-Wah'
_publ_section_title
;
 Syntheses, photophysical, electroluminescence and computational studies
 of rhenium(i) diimine triarylamine-containing alkynyl complexes
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1753
_journal_paper_doi               10.1039/c3nj00121k
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         '2(C37 H22 N3 O3 Re), C4 H10 O'
_chemical_formula_sum            'C78 H54 N6 O7 Re2'
_chemical_formula_weight         1559.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.363(3)
_cell_length_b                   18.607(4)
_cell_length_c                   11.891(2)
_cell_measurement_reflns_used    24568
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      1.74
_cell_volume                     3318.5(12)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1995)'
_computing_data_collection       'Mar data collection software (1996)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Mar imaging plate system'
_diffrn_measurement_method       'φ 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  0.0397
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24568
_diffrn_reflns_theta_full        25.53
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.015
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0298
_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)+(0.0396P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0766
_reflns_number_gt                4812
_reflns_number_total             5827
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c3nj00121k.txt
_cod_data_source_block           mar1672a
_cod_original_sg_symbol_Hall     ' -P 2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7053053
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.495809(10) 0.271159(7) 0.852441(13) 0.03634(7) Uani 1 1 d . . .
O1 O 0.3215(3) 0.2786(2) 0.9412(4) 0.0812(13) Uani 1 1 d . . .
O2 O 0.4202(3) 0.14987(18) 0.6867(3) 0.0761(11) Uani 1 1 d . . .
O3 O 0.5807(2) 0.15355(17) 1.0238(3) 0.0616(9) Uani 1 1 d . . .
O4 O 0.0000 0.5000 0.0000 0.238(6) Uiso 1 2 d S . .
N1 N 0.5520(2) 0.36714(16) 0.9454(3) 0.0389(7) Uani 1 1 d . . .
N2 N 0.4572(2) 0.35998(17) 0.7329(3) 0.0369(7) Uani 1 1 d . . .
N3 N 1.0477(3) 0.2890(2) 0.7195(5) 0.0731(13) Uani 1 1 d . . .
C1 C 0.3839(3) 0.2798(3) 0.9102(4) 0.0523(12) Uani 1 1 d . . .
C2 C 0.4481(3) 0.1956(2) 0.7499(4) 0.0506(11) Uani 1 1 d . . .
C3 C 0.5467(3) 0.1977(2) 0.9628(4) 0.0455(10) Uani 1 1 d . . .
C4 C 0.5982(3) 0.3678(2) 1.0555(4) 0.0494(11) Uani 1 1 d . . .
H4 H 0.5992 0.3262 1.0992 0.059 Uiso 1 1 calc R . .
C5 C 0.6438(3) 0.4266(3) 1.1061(4) 0.0652(13) Uani 1 1 d . . .
H5 H 0.6756 0.4251 1.1821 0.078 Uiso 1 1 calc R . .
C6 C 0.6413(4) 0.4881(3) 1.0417(4) 0.0720(15) Uani 1 1 d . . .
H6 H 0.6714 0.5291 1.0739 0.086 Uiso 1 1 calc R . .
C7 C 0.5939(3) 0.4889(2) 0.9293(4) 0.0592(12) Uani 1 1 d . . .
H7 H 0.5919 0.5303 0.8850 0.071 Uiso 1 1 calc R . .
C8 C 0.5498(3) 0.4280(2) 0.8831(3) 0.0420(9) Uani 1 1 d . . .
C9 C 0.4944(3) 0.42506(19) 0.7654(3) 0.0387(9) Uani 1 1 d . . .
C10 C 0.4764(3) 0.4827(2) 0.6920(4) 0.0517(11) Uani 1 1 d . . .
H10 H 0.5016 0.5272 0.7152 0.062 Uiso 1 1 calc R . .
C11 C 0.4216(3) 0.4758(2) 0.5847(4) 0.0553(12) Uani 1 1 d . . .
H11 H 0.4101 0.5149 0.5350 0.066 Uiso 1 1 calc R . .
C12 C 0.3847(3) 0.4107(2) 0.5525(4) 0.0520(11) Uani 1 1 d . . .
H12 H 0.3471 0.4045 0.4805 0.062 Uiso 1 1 calc R . .
C13 C 0.4038(3) 0.3538(2) 0.6285(3) 0.0449(10) Uani 1 1 d . . .
H13 H 0.3784 0.3093 0.6060 0.054 Uiso 1 1 calc R . .
C14 C 0.6221(3) 0.27147(19) 0.7967(4) 0.0392(9) Uani 1 1 d . . .
C15 C 0.6894(3) 0.2742(2) 0.7773(4) 0.0483(11) Uani 1 1 d . . .
C16 C 0.7809(3) 0.2786(2) 0.7593(4) 0.0518(11) Uani 1 1 d . . .
C17 C 0.8081(4) 0.2440(3) 0.6689(6) 0.086(2) Uani 1 1 d . . .
H17 H 0.7669 0.2172 0.6166 0.104 Uiso 1 1 calc R . .
C18 C 0.8953(4) 0.2488(4) 0.6551(6) 0.0843(19) Uani 1 1 d . . .
H18 H 0.9115 0.2265 0.5927 0.101 Uiso 1 1 calc R . .
C19 C 0.9574(3) 0.2861(3) 0.7327(5) 0.0623(13) Uani 1 1 d . . .
C20 C 0.9323(4) 0.3221(4) 0.8214(5) 0.0833(18) Uani 1 1 d . . .
H20 H 0.9739 0.3494 0.8724 0.100 Uiso 1 1 calc R . .
C21 C 0.8454(3) 0.3179(3) 0.8353(5) 0.0739(15) Uani 1 1 d . . .
H21 H 0.8296 0.3418 0.8966 0.089 Uiso 1 1 calc R . .
C22 C 1.0979(3) 0.2237(2) 0.7347(5) 0.0604(13) Uani 1 1 d . . .
C23 C 1.0936(4) 0.1786(3) 0.8259(5) 0.0728(15) Uani 1 1 d . . .
H23 H 1.0591 0.1913 0.8782 0.087 Uiso 1 1 calc R . .
C24 C 1.1408(3) 0.1146(3) 0.8394(4) 0.0689(14) Uani 1 1 d . . .
H24 H 1.1371 0.0845 0.9006 0.083 Uiso 1 1 calc R . .
C25 C 1.1927(3) 0.0947(3) 0.7643(4) 0.0609(12) Uani 1 1 d . . .
C26 C 1.1980(4) 0.1401(3) 0.6731(5) 0.0713(14) Uani 1 1 d . . .
H26 H 1.2334 0.1274 0.6219 0.086 Uiso 1 1 calc R . .
C27 C 1.1504(4) 0.2047(3) 0.6577(5) 0.0663(14) Uani 1 1 d . . .
H27 H 1.1538 0.2348 0.5964 0.080 Uiso 1 1 calc R . .
C28 C 1.2416(4) 0.0275(3) 0.7788(5) 0.0723(14) Uani 1 1 d . . .
C29 C 1.2792(4) -0.0274(3) 0.7922(5) 0.0860(17) Uani 1 1 d . . .
H29 H 1.3091 -0.0711 0.8029 0.103 Uiso 1 1 calc R . .
C30 C 1.0851(3) 0.3554(3) 0.6959(4) 0.0586(12) Uani 1 1 d . . .
C31 C 1.1758(3) 0.3664(3) 0.7191(4) 0.0580(12) Uani 1 1 d . . .
H31 H 1.2142 0.3299 0.7526 0.070 Uiso 1 1 calc R . .
C32 C 1.2097(3) 0.4308(3) 0.6930(4) 0.0604(12) Uani 1 1 d . . .
H32 H 1.2713 0.4364 0.7079 0.072 Uiso 1 1 calc R . .
C33 C 1.1565(4) 0.4877(3) 0.6457(4) 0.0601(12) Uani 1 1 d . . .
C34 C 1.0642(4) 0.4771(3) 0.6266(5) 0.0746(15) Uani 1 1 d . . .
H34 H 1.0260 0.5147 0.5975 0.089 Uiso 1 1 calc R . .
C35 C 1.0284(3) 0.4120(3) 0.6498(4) 0.0697(15) Uani 1 1 d . . .
H35 H 0.9669 0.4058 0.6350 0.084 Uiso 1 1 calc R . .
C36 C 1.1919(4) 0.5545(3) 0.6162(4) 0.0720(15) Uani 1 1 d . . .
C37 C 1.2227(5) 0.6082(4) 0.5920(6) 0.098(2) Uani 1 1 d . . .
H37 H 1.2473 0.6509 0.5727 0.117 Uiso 1 1 calc R . .
C38' C -0.0860(14) 0.5002(11) 0.0300(16) 0.148(7) Uiso 0.50 1 d P A 2
H38A H -0.0904 0.5447 0.0708 0.177 Uiso 0.50 1 calc PR A 2
H38B H -0.1305 0.5024 -0.0414 0.177 Uiso 0.50 1 calc PR A 2
C38 C -0.0215(13) 0.4645(12) 0.0817(18) 0.156(7) Uiso 0.50 1 d P A 1
H38C H 0.0066 0.4876 0.1535 0.187 Uiso 0.50 1 calc PR A 1
H38D H 0.0046 0.4170 0.0822 0.187 Uiso 0.50 1 calc PR A 1
C39 C -0.1058(10) 0.4563(9) 0.0821(12) 0.248(7) Uiso 1 1 d . . .
H39D H -0.0588 0.4213 0.0991 0.298 Uiso 0.50 1 calc PR A 2
H39E H -0.1591 0.4338 0.0395 0.298 Uiso 0.50 1 calc PR A 2
H39F H -0.1166 0.4755 0.1527 0.298 Uiso 0.50 1 calc PR A 2
H39A H -0.1174 0.4057 0.0861 0.298 Uiso 0.50 1 d PR A 1
H39B H -0.1427 0.4759 0.0134 0.298 Uiso 0.50 1 d PR A 1
H39C H -0.1188 0.4799 0.1482 0.298 Uiso 0.50 1 d PR A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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'
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
C2 Re1 C3 87.5(2) . .
C2 Re1 C1 92.2(2) . .
C3 Re1 C1 94.30(17) . .
C2 Re1 N2 97.48(17) . .
C3 Re1 N2 172.03(15) . .
C1 Re1 N2 91.76(14) . .
C2 Re1 N1 170.90(15) . .
C3 Re1 N1 100.22(16) . .
C1 Re1 N1 92.07(17) . .
N2 Re1 N1 74.37(12) . .
C2 Re1 C14 92.98(17) . .
C3 Re1 C14 87.27(16) . .
C1 Re1 C14 174.62(18) . .
N2 Re1 C14 86.23(13) . .
N1 Re1 C14 82.58(13) . .
C38 O4 C38 180.0(17) . 3_565
C38 O4 C38' 126.1(10) . 3_565
C38 O4 C38' 53.9(10) 3_565 3_565
C38 O4 C38' 53.9(10) . .
C38 O4 C38' 126.1(10) 3_565 .
C38' O4 C38' 180.0(4) 3_565 .
C4 N1 C8 118.1(4) . .
C4 N1 Re1 124.6(3) . .
C8 N1 Re1 116.7(2) . .
C13 N2 C9 118.4(3) . .
C13 N2 Re1 124.5(3) . .
C9 N2 Re1 116.9(3) . .
C30 N3 C22 122.4(4) . .
C30 N3 C19 120.0(4) . .
C22 N3 C19 117.6(4) . .
O1 C1 Re1 174.2(5) . .
O2 C2 Re1 178.9(4) . .
O3 C3 Re1 175.6(4) . .
N1 C4 C5 123.1(4) . .
C4 C5 C6 118.2(4) . .
C5 C6 C7 119.7(5) . .
C8 C7 C6 119.4(4) . .
N1 C8 C7 121.5(4) . .
N1 C8 C9 115.5(3) . .
C7 C8 C9 122.9(4) . .
N2 C9 C10 120.1(4) . .
N2 C9 C8 115.1(3) . .
C10 C9 C8 124.8(4) . .
C9 C10 C11 121.0(4) . .
C12 C11 C10 118.7(4) . .
C11 C12 C13 118.9(4) . .
N2 C13 C12 122.9(4) . .
C15 C14 Re1 174.0(4) . .
C14 C15 C16 176.4(6) . .
C17 C16 C21 116.9(5) . .
C17 C16 C15 122.9(5) . .
C21 C16 C15 120.2(4) . .
C18 C17 C16 121.4(5) . .
C19 C18 C17 120.3(5) . .
C18 C19 C20 119.7(5) . .
C18 C19 N3 119.8(5) . .
C20 C19 N3 120.4(5) . .
C19 C20 C21 120.2(5) . .
C20 C21 C16 121.5(5) . .
C23 C22 C27 119.6(5) . .
C23 C22 N3 119.9(5) . .
C27 C22 N3 120.4(5) . .
C22 C23 C24 120.0(5) . .
C25 C24 C23 121.4(5) . .
C24 C25 C26 119.0(5) . .
C24 C25 C28 121.0(5) . .
C26 C25 C28 120.0(5) . .
C25 C26 C27 120.4(5) . .
C22 C27 C26 119.6(5) . .
C29 C28 C25 177.9(7) . .
C31 C30 C35 119.0(5) . .
C31 C30 N3 121.8(5) . .
C35 C30 N3 119.2(4) . .
C32 C31 C30 120.2(5) . .
C31 C32 C33 122.9(5) . .
C32 C33 C34 116.5(5) . .
C32 C33 C36 123.0(5) . .
C34 C33 C36 120.6(5) . .
C35 C34 C33 121.6(5) . .
C34 C35 C30 119.7(5) . .
C37 C36 C33 178.3(7) . .
C39 C38' O4 121(2) . .
O4 C38 C39 119.0(19) . .
C38' C39 C38 61.2(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C2 1.901(5) .
Re1 C3 1.938(5) .
Re1 C1 1.992(5) .
Re1 N2 2.176(3) .
Re1 N1 2.178(3) .
Re1 C14 2.182(5) .
O1 C1 1.099(6) .
O2 C2 1.154(6) .
O3 C3 1.145(5) .
O4 C38 1.28(2) .
O4 C38 1.28(2) 3_565
O4 C38' 1.441(19) 3_565
O4 C38' 1.441(19) .
N1 C4 1.348(5) .
N1 C8 1.349(5) .
N2 C13 1.337(5) .
N2 C9 1.359(5) .
N3 C30 1.417(6) .
N3 C22 1.430(6) .
N3 C19 1.430(6) .
C4 C5 1.368(7) .
C5 C6 1.373(7) .
C6 C7 1.377(6) .
C7 C8 1.373(6) .
C8 C9 1.473(5) .
C9 C10 1.373(6) .
C10 C11 1.374(6) .
C11 C12 1.357(6) .
C12 C13 1.381(6) .
C14 C15 1.107(6) .
C15 C16 1.469(7) .
C16 C17 1.393(7) .
C16 C21 1.395(7) .
C17 C18 1.387(7) .
C18 C19 1.365(8) .
C19 C20 1.373(7) .
C20 C21 1.383(7) .
C22 C23 1.384(7) .
C22 C27 1.390(7) .
C23 C24 1.385(7) .
C24 C25 1.370(7) .
C25 C26 1.392(7) .
C25 C28 1.449(7) .
C26 C27 1.398(7) .
C28 C29 1.167(7) .
C30 C31 1.375(6) .
C30 C35 1.401(7) .
C31 C32 1.368(7) .
C32 C33 1.382(7) .
C33 C34 1.402(7) .
C33 C36 1.429(7) .
C34 C35 1.382(8) .
C36 C37 1.168(8) .
C38' C39 1.11(2) .
C38 C39 1.305(19) .
