#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/30/7053055.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_7053055
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         'C41 H38 N3 O3 Re, 2(C H2 Cl2)'
_chemical_formula_sum            'C43 H42 Cl4 N3 O3 Re'
_chemical_formula_weight         976.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 124.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.572(7)
_cell_length_b                   12.522(3)
_cell_length_c                   23.379(5)
_cell_measurement_reflns_used    25191
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      1.75
_cell_volume                     8795(5)
_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      301(2)
_diffrn_measured_fraction_theta_full 0.885
_diffrn_measured_fraction_theta_max 0.885
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25191
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.173
_refine_diff_density_min         -2.015
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0443
_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)+(0.0667P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                4789
_reflns_number_total             7207
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c3nj00121k.txt
_cod_data_source_block           mar1395
_cod_original_cell_volume        8795(3)
_cod_original_sg_symbol_Hall     ' -C 2yc'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7053055
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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 0.241875(10) 0.940798(18) 0.857875(14) 0.04789(12) Uani 1 1 d .
O1 O 0.3081(2) 1.0969(5) 0.9751(3) 0.105(2) Uani 1 1 d .
O2 O 0.1731(2) 1.1200(4) 0.7907(3) 0.0851(18) Uani 1 1 d .
O3 O 0.2050(2) 0.8763(5) 0.9422(3) 0.099(2) Uani 1 1 d .
N1 N 0.28991(17) 0.8115(4) 0.8899(3) 0.0477(13) Uani 1 1 d .
N2 N 0.26837(18) 0.9563(4) 0.7953(3) 0.0461(13) Uani 1 1 d .
N3 N 0.0662(2) 0.4457(4) 0.5367(3) 0.0663(17) Uani 1 1 d .
C1 C 0.2844(3) 1.0384(6) 0.9315(4) 0.065(2) Uani 1 1 d .
C2 C 0.1990(3) 1.0524(6) 0.8171(4) 0.0605(19) Uani 1 1 d .
C3 C 0.2185(3) 0.9017(6) 0.9104(4) 0.067(2) Uani 1 1 d .
C4 C 0.1963(2) 0.8328(5) 0.7773(4) 0.0525(17) Uani 1 1 d .
C5 C 0.1719(2) 0.7706(5) 0.7321(4) 0.0563(18) Uani 1 1 d .
C6 C 0.1429(2) 0.6946(5) 0.6798(4) 0.0550(17) Uani 1 1 d .
C7 C 0.1502(2) 0.6610(5) 0.6312(4) 0.0634(19) Uani 1 1 d .
H7 H 0.1724 0.6941 0.6296 0.076 Uiso 1 1 calc R
C8 C 0.1257(2) 0.5795(5) 0.5846(4) 0.0581(18) Uani 1 1 d .
H8 H 0.1321 0.5573 0.5533 0.070 Uiso 1 1 calc R
C9 C 0.0912(3) 0.5304(5) 0.5845(4) 0.061(2) Uani 1 1 d .
C10 C 0.0828(2) 0.5659(5) 0.6319(4) 0.065(2) Uani 1 1 d .
H10 H 0.0595 0.5360 0.6317 0.078 Uiso 1 1 calc R
C11 C 0.1088(2) 0.6458(5) 0.6801(4) 0.0592(18) Uani 1 1 d .
H11 H 0.1032 0.6667 0.7127 0.071 Uiso 1 1 calc R
C12 C 0.0490(2) 0.3601(5) 0.5535(4) 0.065(2) Uani 1 1 d .
C13 C 0.0692(3) 0.3263(6) 0.6223(4) 0.073(2) Uani 1 1 d .
H13 H 0.0951 0.3587 0.6586 0.087 Uiso 1 1 calc R
C14 C 0.0504(3) 0.2461(7) 0.6349(5) 0.094(3) Uani 1 1 d .
H14 H 0.0634 0.2244 0.6807 0.113 Uiso 1 1 calc R
C15 C 0.0127(4) 0.1951(7) 0.5828(7) 0.105(3) Uani 1 1 d .
H15 H 0.0004 0.1404 0.5936 0.126 Uiso 1 1 calc R
C16 C -0.0069(3) 0.2244(7) 0.5150(6) 0.101(3) Uani 1 1 d .
H16 H -0.0322 0.1894 0.4794 0.121 Uiso 1 1 calc R
C17 C 0.0114(3) 0.3059(6) 0.5005(5) 0.081(2) Uani 1 1 d .
H17 H -0.0014 0.3256 0.4544 0.097 Uiso 1 1 calc R
C18 C 0.0614(3) 0.4453(5) 0.4725(4) 0.065(2) Uani 1 1 d .
C19 C 0.0810(3) 0.3638(7) 0.4578(5) 0.101(3) Uani 1 1 d .
H19 H 0.0964 0.3092 0.4898 0.122 Uiso 1 1 calc R
C20 C 0.0774(5) 0.3645(10) 0.3957(7) 0.145(5) Uani 1 1 d .
H20 H 0.0903 0.3098 0.3859 0.174 Uiso 1 1 calc R
C21 C 0.0551(5) 0.4450(12) 0.3485(6) 0.138(5) Uani 1 1 d .
H21 H 0.0534 0.4455 0.3073 0.166 Uiso 1 1 calc R
C22 C 0.0348(4) 0.5264(10) 0.3617(6) 0.114(4) Uani 1 1 d .
H22 H 0.0191 0.5801 0.3291 0.137 Uiso 1 1 calc R
C23 C 0.0384(3) 0.5261(7) 0.4240(5) 0.086(3) Uani 1 1 d .
H23 H 0.0254 0.5806 0.4335 0.103 Uiso 1 1 calc R
C24 C 0.3021(2) 0.7439(5) 0.9427(3) 0.0560(18) Uani 1 1 d .
H24 H 0.2918 0.7563 0.9703 0.067 Uiso 1 1 calc R
C25 C 0.3291(2) 0.6577(5) 0.9575(4) 0.0626(19) Uani 1 1 d .
H25 H 0.3364 0.6130 0.9944 0.075 Uiso 1 1 calc R
C26 C 0.3457(2) 0.6362(5) 0.9180(3) 0.0518(17) Uani 1 1 d .
C27 C 0.3337(2) 0.7088(5) 0.8647(3) 0.0514(17) Uani 1 1 d .
H27 H 0.3444 0.6992 0.8373 0.062 Uiso 1 1 calc R
C28 C 0.3066(2) 0.7937(5) 0.8518(3) 0.0444(15) Uani 1 1 d .
C29 C 0.2933(2) 0.8741(5) 0.7960(3) 0.0449(15) Uani 1 1 d .
C30 C 0.3052(2) 0.8700(5) 0.7506(3) 0.0482(16) Uani 1 1 d .
H30 H 0.3215 0.8118 0.7520 0.058 Uiso 1 1 calc R
C31 C 0.2937(2) 0.9502(5) 0.7021(3) 0.0507(16) Uani 1 1 d .
C32 C 0.2702(2) 1.0367(5) 0.7042(4) 0.0568(18) Uani 1 1 d .
H32 H 0.2629 1.0947 0.6747 0.068 Uiso 1 1 calc R
C33 C 0.2579(2) 1.0358(5) 0.7498(4) 0.0521(17) Uani 1 1 d .
H33 H 0.2415 1.0932 0.7492 0.063 Uiso 1 1 calc R
C34 C 0.3758(3) 0.5398(5) 0.9353(4) 0.065(2) Uani 1 1 d .
C35 C 0.3525(4) 0.4377(6) 0.9362(6) 0.113(4) Uani 1 1 d .
H35A H 0.3715 0.3772 0.9469 0.169 Uiso 1 1 calc R
H35B H 0.3251 0.4278 0.8914 0.169 Uiso 1 1 calc R
H35C H 0.3464 0.4446 0.9710 0.169 Uiso 1 1 calc R
C36 C 0.4185(3) 0.5557(6) 1.0064(5) 0.109(4) Uani 1 1 d .
H36A H 0.4377 0.4953 1.0177 0.164 Uiso 1 1 calc R
H36B H 0.4119 0.5628 1.0405 0.164 Uiso 1 1 calc R
H36C H 0.4332 0.6192 1.0062 0.164 Uiso 1 1 calc R
C37 C 0.3877(4) 0.5234(8) 0.8838(5) 0.116(4) Uani 1 1 d .
H37A H 0.4065 0.4617 0.8970 0.174 Uiso 1 1 calc R
H37B H 0.4032 0.5852 0.8836 0.174 Uiso 1 1 calc R
H37C H 0.3610 0.5128 0.8382 0.174 Uiso 1 1 calc R
C38 C 0.3051(3) 0.9441(5) 0.6485(4) 0.063(2) Uani 1 1 d .
C39 C 0.2715(3) 0.8680(8) 0.5915(4) 0.112(4) Uani 1 1 d .
H39A H 0.2420 0.8952 0.5707 0.168 Uiso 1 1 calc R
H39B H 0.2740 0.7990 0.6114 0.168 Uiso 1 1 calc R
H39C H 0.2775 0.8618 0.5566 0.168 Uiso 1 1 calc R
C40 C 0.3517(3) 0.9025(7) 0.6818(4) 0.087(3) Uani 1 1 d .
H40A H 0.3582 0.8986 0.6475 0.131 Uiso 1 1 calc R
H40B H 0.3540 0.8326 0.7005 0.131 Uiso 1 1 calc R
H40C H 0.3724 0.9497 0.7186 0.131 Uiso 1 1 calc R
C41 C 0.3018(4) 1.0537(6) 0.6165(5) 0.099(3) Uani 1 1 d .
H41A H 0.2724 1.0819 0.5953 0.148 Uiso 1 1 calc R
H41B H 0.3079 1.0462 0.5818 0.148 Uiso 1 1 calc R
H41C H 0.3231 1.1016 0.6523 0.148 Uiso 1 1 calc R
C42 C 0.1005(9) 1.226(3) 0.9009(14) 0.51(3) Uiso 1 1 d D
H42A H 0.0958 1.2137 0.9372 0.611 Uiso 1 1 calc R
H42B H 0.1076 1.3008 0.9002 0.611 Uiso 1 1 calc R
C43 C 0.0626(11) 0.9798(19) 0.7504(12) 0.51(2) Uiso 1 1 d D
H43A H 0.0826 1.0331 0.7525 0.618 Uiso 1 1 calc R
H43B H 0.0417 1.0116 0.7585 0.618 Uiso 1 1 calc R
Cl3 Cl 0.0898(4) 0.8652(11) 0.8012(6) 0.505(7) Uiso 1 1 d D
Cl4 Cl 0.0362(3) 0.8926(9) 0.6721(5) 0.393(5) Uiso 1 1 d D
Cl1 Cl 0.1399(5) 1.1340(12) 0.9035(8) 0.564(8) Uiso 1 1 d D
Cl2 Cl 0.0567(5) 1.1770(11) 0.8180(8) 0.559(8) Uiso 1 1 d D
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'
Cl Cl 0.1484 0.1585 '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
C2 Re1 C3 88.2(3)
C2 Re1 C1 89.8(3)
C3 Re1 C1 91.0(3)
C2 Re1 C4 91.0(3)
C3 Re1 C4 89.7(3)
C1 Re1 C4 178.9(3)
C2 Re1 N2 98.8(2)
C3 Re1 N2 170.3(2)
C1 Re1 N2 95.7(2)
C4 Re1 N2 83.5(2)
C2 Re1 N1 171.5(2)
C3 Re1 N1 99.0(3)
C1 Re1 N1 94.6(3)
C4 Re1 N1 84.5(2)
N2 Re1 N1 73.56(18)
C24 N1 C28 117.4(5)
C24 N1 Re1 124.3(4)
C28 N1 Re1 118.2(4)
C33 N2 C29 117.0(5)
C33 N2 Re1 124.3(4)
C29 N2 Re1 118.3(4)
C12 N3 C18 119.4(6)
C12 N3 C9 122.3(6)
C18 N3 C9 118.2(6)
O1 C1 Re1 177.3(7)
O2 C2 Re1 178.0(6)
O3 C3 Re1 178.6(7)
C5 C4 Re1 177.9(6)
C4 C5 C6 178.4(7)
C7 C6 C11 117.9(6)
C7 C6 C5 120.7(7)
C11 C6 C5 121.1(7)
C6 C7 C8 122.1(7)
C7 C8 C9 120.2(7)
C10 C9 C8 118.0(7)
C10 C9 N3 122.0(7)
C8 C9 N3 120.0(7)
C9 C10 C11 121.2(7)
C6 C11 C10 120.5(7)
C17 C12 C13 118.7(8)
C17 C12 N3 119.6(8)
C13 C12 N3 121.7(7)
C14 C13 C12 118.6(8)
C13 C14 C15 122.4(9)
C16 C15 C14 120.2(9)
C15 C16 C17 118.8(9)
C16 C17 C12 121.2(9)
C23 C18 C19 119.2(8)
C23 C18 N3 121.0(8)
C19 C18 N3 119.7(7)
C20 C19 C18 120.0(9)
C21 C20 C19 120.5(11)
C20 C21 C22 120.5(11)
C23 C22 C21 119.1(11)
C22 C23 C18 120.6(10)
N1 C24 C25 123.0(6)
C24 C25 C26 120.7(6)
C25 C26 C27 115.5(6)
C25 C26 C34 120.0(6)
C27 C26 C34 124.5(6)
C28 C27 C26 121.6(6)
N1 C28 C27 121.8(5)
N1 C28 C29 114.8(5)
C27 C28 C29 123.4(6)
C30 C29 N2 121.8(5)
C30 C29 C28 124.6(6)
N2 C29 C28 113.5(5)
C29 C30 C31 121.9(6)
C30 C31 C32 115.9(6)
C30 C31 C38 122.3(6)
C32 C31 C38 121.7(6)
C33 C32 C31 120.0(6)
N2 C33 C32 123.3(6)
C37 C34 C36 107.9(8)
C37 C34 C26 112.9(6)
C36 C34 C26 109.0(6)
C37 C34 C35 108.1(7)
C36 C34 C35 109.1(7)
C26 C34 C35 109.8(7)
C40 C38 C39 110.2(7)
C40 C38 C31 110.5(6)
C39 C38 C31 106.6(6)
C40 C38 C41 108.2(7)
C39 C38 C41 109.4(7)
C31 C38 C41 111.9(6)
Cl2 C42 Cl1 91.1(11)
Cl3 C43 Cl4 87.8(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C2 1.901(8)
Re1 C3 1.916(8)
Re1 C1 1.956(8)
Re1 C4 2.139(7)
Re1 N2 2.175(5)
Re1 N1 2.183(5)
O1 C1 1.149(8)
O2 C2 1.153(8)
O3 C3 1.150(8)
N1 C24 1.345(7)
N1 C28 1.354(7)
N2 C33 1.344(7)
N2 C29 1.370(7)
N3 C12 1.408(9)
N3 C18 1.408(9)
N3 C9 1.429(8)
C4 C5 1.202(9)
C5 C6 1.431(9)
C6 C7 1.374(9)
C6 C11 1.392(9)
C7 C8 1.385(9)
C8 C9 1.402(10)
C9 C10 1.382(10)
C10 C11 1.398(9)
C12 C17 1.394(10)
C12 C13 1.399(10)
C13 C14 1.342(10)
C14 C15 1.370(13)
C15 C16 1.365(13)
C16 C17 1.366(11)
C18 C23 1.389(10)
C18 C19 1.396(11)
C19 C20 1.381(13)
C20 C21 1.369(15)
C21 C22 1.394(15)
C22 C23 1.386(13)
C24 C25 1.367(9)
C25 C26 1.391(9)
C26 C27 1.396(8)
C26 C34 1.523(9)
C27 C28 1.365(8)
C28 C29 1.493(8)
C29 C30 1.360(8)
C30 C31 1.388(8)
C31 C32 1.401(8)
C31 C38 1.531(9)
C32 C33 1.374(9)
C34 C37 1.509(11)
C34 C36 1.510(11)
C34 C35 1.544(10)
C38 C40 1.505(11)
C38 C39 1.525(11)
C38 C41 1.535(9)
C42 Cl2 1.779(18)
C42 Cl1 1.821(18)
C43 Cl3 1.764(19)
C43 Cl4 1.860(19)
