#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:18:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179784 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/80/7008060.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_7008060
loop_
_publ_author_name
'Lazarides, Theodore'
'Miller, Thomas A.'
'Jeffery, John C.'
'Ronson, Tanya K.'
'Adams, Harry'
'Ward, Michael D.'
_publ_section_title
;
 Luminescent complexes of Re(I) and Ru(II) with appended macrocycle
 groups derived from 5,6-dihydroxyphenanthroline: cation and anion
 binding.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              528
_journal_page_last               536
_journal_paper_doi               10.1039/b416293e
_journal_year                    2005
_chemical_formula_sum            'C33 H34 Cl N2 O11 Re'
_chemical_formula_weight         856.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 97.565(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.4640(7)
_cell_length_b                   13.3917(4)
_cell_length_c                   11.4092(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3250.91(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16284
_diffrn_reflns_theta_full        67.83
_diffrn_reflns_theta_max         67.83
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    8.628
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.02
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.761
_refine_diff_density_min         -2.142
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5068
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0672
_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)+(0.0000P)²+70.0064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                5010
_reflns_number_total             5068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b416293e.txt
_cod_data_source_block           ted
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7008060
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
Re Re 0.37431(2) 0.63072(4) 0.21791(4) 0.01901(17) Uani 1 1 d D . .
C41 C 0.3165(5) 0.6513(8) 0.0721(10) 0.023(2) Uani 1 1 d . A .
O41 O 0.2870(4) 0.6669(7) -0.0148(7) 0.033(2) Uani 1 1 d . . .
C42 C 0.3048(5) 0.6298(9) 0.3109(10) 0.023(2) Uani 1 1 d . A .
O42 O 0.2643(4) 0.6215(6) 0.3651(7) 0.0299(19) Uani 1 1 d . . .
C43 C 0.3638(9) 0.4854(14) 0.2004(16) 0.025 Uiso 0.766(13) 1 d PDU A 1
C43A C 0.390(3) 0.776(2) 0.224(7) 0.025 Uiso 0.234(13) 1 d PDU A 2
O43 O 0.3575(5) 0.3995(8) 0.1942(8) 0.024(2) Uiso 0.766(13) 1 d PDU A 1
O43A O 0.3862(17) 0.861(2) 0.240(3) 0.025 Uiso 0.234(13) 1 d PDU A 2
Cl Cl 0.38746(17) 0.8098(3) 0.2378(3) 0.0147(12) Uani 0.766(13) 1 d PDU A 1
ClA Cl 0.3726(6) 0.4583(7) 0.2017(11) 0.016(4) Uiso 0.234(13) 1 d PDU A 2
N1 N 0.4508(4) 0.6232(6) 0.3646(7) 0.0134(17) Uani 1 1 d . A .
C2 C 0.4462(5) 0.6215(7) 0.4791(8) 0.014(2) Uani 1 1 d . . .
H12 H 0.4056 0.6211 0.5037 0.017 Uiso 1 1 calc R A .
C3 C 0.4989(5) 0.6201(7) 0.5651(8) 0.014(2) Uani 1 1 d . A .
H11 H 0.4936 0.6201 0.6465 0.017 Uiso 1 1 calc R . .
C4 C 0.5578(5) 0.6188(7) 0.5328(9) 0.017(2) Uani 1 1 d . . .
H24 H 0.5937 0.6169 0.5912 0.020 Uiso 1 1 calc R A .
C5 C 0.5649(5) 0.6204(7) 0.4121(9) 0.015(2) Uani 1 1 d . A .
C6 C 0.5101(5) 0.6247(6) 0.3311(8) 0.011(2) Uani 1 1 d . . .
C7 C 0.5143(5) 0.6267(7) 0.2077(9) 0.014(2) Uani 1 1 d . A .
N8 N 0.4594(4) 0.6306(6) 0.1318(7) 0.0149(18) Uani 1 1 d . A .
C9 C 0.4624(5) 0.6311(7) 0.0161(9) 0.018(2) Uani 1 1 d . . .
H16 H 0.4245 0.6337 -0.0372 0.022 Uiso 1 1 calc R A .
C10 C 0.5198(5) 0.6280(7) -0.0292(9) 0.018(2) Uani 1 1 d . A .
H19 H 0.5202 0.6266 -0.1123 0.021 Uiso 1 1 calc R . .
C11 C 0.5753(5) 0.6269(7) 0.0447(9) 0.017(2) Uani 1 1 d . . .
H25 H 0.6144 0.6266 0.0141 0.021 Uiso 1 1 calc R A .
C12 C 0.5729(5) 0.6264(7) 0.1678(9) 0.014(2) Uani 1 1 d . A .
C13 C 0.6288(5) 0.6300(8) 0.2515(10) 0.024(2) Uiso 1 1 d . . .
C14 C 0.6255(5) 0.6185(8) 0.3716(9) 0.020(2) Uani 1 1 d . A .
O15 O 0.6757(3) 0.6060(6) 0.4540(6) 0.0224(16) Uani 1 1 d . . .
C16 C 0.7200(5) 0.6898(9) 0.4707(10) 0.026(3) Uani 1 1 d . A .
H10A H 0.7023 0.7443 0.5149 0.031 Uiso 1 1 calc R . .
H10B H 0.7282 0.7162 0.3932 0.031 Uiso 1 1 calc R . .
C17 C 0.7790(5) 0.6520(9) 0.5383(10) 0.028(3) Uani 1 1 d . . .
H26A H 0.8053 0.7090 0.5706 0.034 Uiso 1 1 calc R A .
H26B H 0.7691 0.6107 0.6053 0.034 Uiso 1 1 calc R . .
O18 O 0.8131(3) 0.5931(6) 0.4622(6) 0.0273(18) Uani 1 1 d . A .
C19 C 0.8709(5) 0.5557(9) 0.5214(10) 0.027(3) Uani 1 1 d . . .
H40A H 0.8629 0.5190 0.5934 0.033 Uiso 1 1 calc R A .
H40B H 0.8994 0.6121 0.5460 0.033 Uiso 1 1 calc R . .
C20 C 0.9012(6) 0.4874(8) 0.4422(10) 0.028(3) Uani 1 1 d . A .
H39A H 0.9364 0.4514 0.4889 0.034 Uiso 1 1 calc R . .
H39B H 0.8703 0.4374 0.4072 0.034 Uiso 1 1 calc R . .
O21 O 0.9244(4) 0.5426(5) 0.3503(7) 0.0254(17) Uani 1 1 d . . .
C22 C 0.9594(5) 0.4794(8) 0.2815(10) 0.026(3) Uani 1 1 d . A .
H41A H 0.9337 0.4207 0.2531 0.031 Uiso 1 1 calc R . .
H41B H 0.9978 0.4552 0.3309 0.031 Uiso 1 1 calc R . .
C23 C 0.9775(6) 0.5379(9) 0.1762(10) 0.029(3) Uani 1 1 d . . .
H38A H 0.9988 0.4932 0.1249 0.035 Uiso 1 1 calc R A .
H38B H 0.9392 0.5650 0.1289 0.035 Uiso 1 1 calc R . .
O24 O 1.0181(4) 0.6169(6) 0.2179(7) 0.0317(19) Uani 1 1 d . A .
C25 C 1.0576(6) 0.6533(7) 0.1433(9) 0.022(2) Uani 1 1 d . . .
C26 C 1.1196(5) 0.6645(8) 0.1872(10) 0.025(3) Uani 1 1 d . A .
H102 H 1.1335 0.6415 0.2650 0.030 Uiso 1 1 calc R . .
C27 C 1.1628(5) 0.7077(8) 0.1233(10) 0.025(3) Uani 1 1 d . . .
H43 H 1.2053 0.7169 0.1568 0.030 Uiso 1 1 calc R A .
C28 C 1.1418(6) 0.7373(9) 0.0080(10) 0.028(3) Uani 1 1 d . A .
H35 H 1.1710 0.7645 -0.0391 0.033 Uiso 1 1 calc R . .
C29 C 1.0799(5) 0.7280(8) -0.0393(10) 0.024(2) Uani 1 1 d . . .
H37 H 1.0667 0.7502 -0.1177 0.029 Uiso 1 1 calc R A .
C30 C 1.0363(6) 0.6862(8) 0.0270(10) 0.025(2) Uani 1 1 d . A .
O31 O 0.9733(4) 0.6781(6) -0.0128(7) 0.0258(17) Uani 1 1 d . . .
C32 C 0.9529(6) 0.7166(9) -0.1282(10) 0.030(3) Uani 1 1 d . A .
H42A H 0.9735 0.6795 -0.1876 0.035 Uiso 1 1 calc R . .
H42B H 0.9646 0.7879 -0.1321 0.035 Uiso 1 1 calc R . .
C33 C 0.8839(5) 0.7055(8) -0.1535(12) 0.032(3) Uani 1 1 d . . .
H8A H 0.8642 0.7315 -0.0860 0.038 Uiso 1 1 calc R A .
H8B H 0.8681 0.7452 -0.2243 0.038 Uiso 1 1 calc R . .
O34 O 0.8666(4) 0.6019(6) -0.1735(7) 0.0321(19) Uani 1 1 d . A .
C35 C 0.8082(5) 0.5766(8) -0.1363(9) 0.022(2) Uani 1 1 d . . .
H32A H 0.7903 0.5167 -0.1789 0.027 Uiso 1 1 calc R A .
H32B H 0.7780 0.6324 -0.1521 0.027 Uiso 1 1 calc R . .
C36 C 0.8215(7) 0.5559(10) -0.0032(11) 0.040(3) Uani 1 1 d . A .
H34A H 0.8426 0.4905 0.0105 0.048 Uiso 1 1 calc R . .
H34B H 0.8497 0.6081 0.0356 0.048 Uiso 1 1 calc R . .
O37 O 0.7660(4) 0.5556(8) 0.0440(7) 0.045(2) Uani 1 1 d . . .
C38 C 0.7776(6) 0.5325(11) 0.1682(10) 0.038(3) Uani 1 1 d . A .
H33A H 0.8033 0.5858 0.2110 0.046 Uiso 1 1 calc R . .
H33B H 0.8007 0.4686 0.1806 0.046 Uiso 1 1 calc R . .
C39 C 0.7158(5) 0.5251(10) 0.2126(10) 0.029(3) Uani 1 1 d . . .
H10C H 0.6885 0.4778 0.1628 0.035 Uiso 1 1 calc R A .
H10D H 0.7218 0.4992 0.2946 0.035 Uiso 1 1 calc R . .
O40 O 0.6858(3) 0.6229(6) 0.2100(6) 0.0229(16) Uani 1 1 d . A .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
C42 Re C41 91.1(5) . . ?
C42 Re C43 87.9(7) . . ?
C41 Re C43 90.1(6) . . ?
C42 Re C43A 97(2) . . ?
C41 Re C43A 89(2) . . ?
C43 Re C43A 175(2) . . ?
C42 Re N8 173.7(4) . . ?
C41 Re N8 95.2(4) . . ?
C43 Re N8 92.6(6) . . ?
C43A Re N8 83(2) . . ?
C42 Re N1 97.8(4) . . ?
C41 Re N1 169.7(4) . . ?
C43 Re N1 95.6(6) . . ?
C43A Re N1 85(2) . . ?
N8 Re N1 75.9(3) . . ?
C42 Re ClA 91.9(5) . . ?
C41 Re ClA 94.1(4) . . ?
C43 Re ClA 5.7(7) . . ?
C43A Re ClA 171(2) . . ?
N8 Re ClA 88.2(4) . . ?
N1 Re ClA 91.0(4) . . ?
C42 Re Cl 92.5(3) . . ?
C41 Re Cl 89.6(3) . . ?
C43 Re Cl 179.5(6) . . ?
C43A Re Cl 5(2) . . ?
N8 Re Cl 87.1(2) . . ?
N1 Re Cl 84.7(2) . . ?
ClA Re Cl 174.2(3) . . ?
O41 C41 Re 174.8(10) . . ?
O42 C42 Re 174.7(10) . . ?
O43 C43 Re 177.7(15) . . ?
O43A C43A Re 164(6) . . ?
C2 N1 C6 117.8(8) . . ?
C2 N1 Re 127.6(7) . . ?
C6 N1 Re 114.5(6) . . ?
N1 C2 C3 122.3(9) . . ?
C4 C3 C2 120.3(9) . . ?
C3 C4 C5 119.2(9) . . ?
C6 C5 C4 117.3(9) . . ?
C6 C5 C14 120.4(9) . . ?
C4 C5 C14 122.3(9) . . ?
N1 C6 C5 123.0(8) . . ?
N1 C6 C7 117.2(8) . . ?
C5 C6 C7 119.8(9) . . ?
N8 C7 C12 122.1(9) . . ?
N8 C7 C6 117.8(9) . . ?
C12 C7 C6 120.1(9) . . ?
C9 N8 C7 118.7(9) . . ?
C9 N8 Re 126.7(7) . . ?
C7 N8 Re 114.6(6) . . ?
N8 C9 C10 121.8(9) . . ?
C11 C10 C9 120.8(9) . . ?
C10 C11 C12 118.1(10) . . ?
C7 C12 C11 118.6(9) . . ?
C7 C12 C13 119.6(9) . . ?
C11 C12 C13 121.8(10) . . ?
O40 C13 C14 119.8(10) . . ?
O40 C13 C12 118.3(9) . . ?
C14 C13 C12 120.4(10) . . ?
O15 C14 C13 124.3(10) . . ?
O15 C14 C5 117.0(9) . . ?
C13 C14 C5 118.8(10) . . ?
C14 O15 C16 116.2(8) . . ?
O15 C16 C17 107.6(9) . . ?
O18 C17 C16 109.9(9) . . ?
C19 O18 C17 112.8(8) . . ?
O18 C19 C20 110.5(9) . . ?
O21 C20 C19 110.5(9) . . ?
C20 O21 C22 110.8(8) . . ?
O21 C22 C23 109.5(8) . . ?
O24 C23 C22 109.2(9) . . ?
C25 O24 C23 117.6(9) . . ?
C26 C25 O24 117.7(10) . . ?
C26 C25 C30 119.3(10) . . ?
O24 C25 C30 122.9(11) . . ?
C25 C26 C27 122.8(10) . . ?
C26 C27 C28 117.5(11) . . ?
C29 C28 C27 121.5(11) . . ?
C28 C29 C30 120.4(11) . . ?
O31 C30 C29 123.7(10) . . ?
O31 C30 C25 117.9(10) . . ?
C29 C30 C25 118.4(11) . . ?
C30 O31 C32 116.4(8) . . ?
O31 C32 C33 108.7(10) . . ?
O34 C33 C32 110.9(9) . . ?
C35 O34 C33 113.7(9) . . ?
O34 C35 C36 106.5(10) . . ?
O37 C36 C35 109.4(11) . . ?
C36 O37 C38 109.9(10) . . ?
O37 C38 C39 107.7(10) . . ?
O40 C39 C38 110.2(10) . . ?
C13 O40 C39 117.8(8) . . ?
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
Re C42 1.941(11) . ?
Re C41 1.959(12) . ?
Re C43 1.967(19) . ?
Re C43A 1.97(3) . ?
Re N8 2.185(8) . ?
Re N1 2.187(8) . ?
Re ClA 2.316(10) . ?
Re Cl 2.421(4) . ?
C41 O41 1.124(13) . ?
C42 O42 1.137(13) . ?
C43 O43 1.16(2) . ?
C43A O43A 1.16(3) . ?
N1 C2 1.324(12) . ?
N1 C6 1.376(13) . ?
C2 C3 1.396(14) . ?
C3 C4 1.364(15) . ?
C4 C5 1.405(14) . ?
C5 C6 1.398(14) . ?
C5 C14 1.437(15) . ?
C6 C7 1.422(13) . ?
C7 N8 1.368(13) . ?
C7 C12 1.394(14) . ?
N8 C9 1.330(13) . ?
C9 C10 1.398(15) . ?
C10 C11 1.366(15) . ?
C11 C12 1.412(14) . ?
C12 C13 1.433(15) . ?
C13 O40 1.373(13) . ?
C13 C14 1.390(15) . ?
C14 O15 1.344(13) . ?
O15 C16 1.467(13) . ?
C16 C17 1.483(16) . ?
C17 O18 1.442(14) . ?
O18 C19 1.422(13) . ?
C19 C20 1.494(16) . ?
C20 O21 1.424(13) . ?
O21 C22 1.434(13) . ?
C22 C23 1.526(16) . ?
C23 O24 1.413(14) . ?
O24 C25 1.369(13) . ?
C25 C26 1.365(16) . ?
C25 C30 1.416(16) . ?
C26 C27 1.380(16) . ?
C27 C28 1.391(17) . ?
C28 C29 1.371(16) . ?
C29 C30 1.397(16) . ?
C30 O31 1.373(13) . ?
O31 C32 1.427(14) . ?
C32 C33 1.479(16) . ?
C33 O34 1.446(13) . ?
O34 C35 1.416(13) . ?
C35 C36 1.533(16) . ?
C36 O37 1.370(16) . ?
O37 C38 1.440(14) . ?
C38 C39 1.484(16) . ?
C39 O40 1.457(14) . ?
