#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050235.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_7050235
loop_
_publ_author_name
'Nail M. Shavaleev'
'Andrea Barbieri'
'Zöe R. Bell'
'Michael D. Ward'
'Francesco Barigelletti'
_publ_section_title
;
 New ligands in the 2,2'-dipyridylamine series and their Re(I)
 complexes; synthesis, structures and luminescence properties
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              398
_journal_page_last               405
_journal_paper_doi               10.1039/b312647a
_journal_volume                  28
_journal_year                    2004
_chemical_formula_moiety         'C33 H39 Cl N3 O10 Re'
_chemical_formula_sum            'C33 H39 Cl N3 O10 Re'
_chemical_formula_weight         859.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.20(3)
_cell_angle_beta                 80.21(4)
_cell_angle_gamma                62.56(2)
_cell_formula_units_Z            2
_cell_length_a                   11.170(4)
_cell_length_b                   11.937(4)
_cell_length_c                   16.536(5)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      1
_cell_measurement_theta_min      0.835189
_cell_volume                     1880.3(12)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1998)'
_computing_data_collection       'Bruker SMART (Bruker, 1998)'
_computing_data_reduction        'Bruker SHELXTL (Bruker, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1998)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'Bruker SHELXTL (Bruker, 1998)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21637
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.357
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.623
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0371
_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)+(0.0278P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                7322
_reflns_number_total             8612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312647a.txt
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1880.3(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050235
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.258276(17) -0.354052(15) 0.328174(11) 0.01270(5) Uani 1 1 d . . .
Cl1 Cl 0.11197(11) -0.29546(10) 0.45350(7) 0.0248(2) Uani 1 1 d . . .
O31 O 0.4959(3) -0.5667(3) 0.4325(2) 0.0272(7) Uani 1 1 d . . .
O41 O 0.1732(3) -0.5630(3) 0.3246(2) 0.0301(8) Uani 1 1 d . . .
O51 O 0.4364(3) -0.4161(3) 0.1711(2) 0.0278(7) Uani 1 1 d . . .
O71 O 0.4402(3) -0.0748(2) -0.10078(17) 0.0146(6) Uani 1 1 d . . .
O74 O 0.4375(3) -0.1814(3) -0.22981(18) 0.0208(7) Uani 1 1 d . . .
O77 O 0.3684(3) -0.0276(3) -0.40407(18) 0.0225(7) Uani 1 1 d . . .
O80 O 0.2531(3) 0.2391(3) -0.41040(18) 0.0214(7) Uani 1 1 d . . .
O83 O 0.2411(3) 0.3604(3) -0.28742(18) 0.0184(6) Uani 1 1 d . . .
O86 O 0.3450(3) 0.1758(2) -0.12945(17) 0.0157(6) Uani 1 1 d . . .
N1 N 0.2386(3) -0.0950(3) 0.1856(2) 0.0141(7) Uani 1 1 d . . .
N11 N 0.3015(3) -0.1931(3) 0.3267(2) 0.0133(7) Uani 1 1 d . . .
N21 N 0.0945(3) -0.1929(3) 0.2557(2) 0.0133(7) Uani 1 1 d . . .
C12 C 0.3089(4) -0.1105(4) 0.2541(3) 0.0152(8) Uani 1 1 d . . .
C13 C 0.3894(4) -0.0464(4) 0.2460(3) 0.0192(9) Uani 1 1 d . . .
H13A H 0.4019 0.0035 0.1942 0.023 Uiso 1 1 calc R . .
C14 C 0.4501(4) -0.0577(4) 0.3152(3) 0.0211(10) Uani 1 1 d . . .
H14A H 0.5064 -0.0178 0.3102 0.025 Uiso 1 1 calc R . .
C15 C 0.4273(4) -0.1287(4) 0.3928(3) 0.0188(9) Uani 1 1 d . . .
H15A H 0.4607 -0.1309 0.4413 0.023 Uiso 1 1 calc R . .
C16 C 0.3539(4) -0.1955(4) 0.3957(3) 0.0154(8) Uani 1 1 d . . .
H16A H 0.3393 -0.2446 0.4472 0.018 Uiso 1 1 calc R . .
C22 C 0.1125(4) -0.1008(4) 0.1943(2) 0.0132(8) Uani 1 1 d . . .
C23 C 0.0115(5) -0.0147(4) 0.1392(3) 0.0216(10) Uani 1 1 d . . .
H23A H 0.0273 0.0443 0.0943 0.026 Uiso 1 1 calc R . .
C24 C -0.1115(5) -0.0174(4) 0.1517(3) 0.0266(11) Uani 1 1 d . . .
H24A H -0.1799 0.0408 0.1155 0.032 Uiso 1 1 calc R . .
C25 C -0.1348(4) -0.1059(4) 0.2178(3) 0.0213(10) Uani 1 1 d . . .
H25A H -0.2188 -0.1071 0.2279 0.026 Uiso 1 1 calc R . .
C26 C -0.0297(4) -0.1918(4) 0.2678(3) 0.0177(9) Uani 1 1 d . . .
H26A H -0.0437 -0.2525 0.3122 0.021 Uiso 1 1 calc R . .
C31 C 0.4051(5) -0.4856(4) 0.3943(3) 0.0186(9) Uani 1 1 d . . .
C41 C 0.2044(4) -0.4839(4) 0.3267(3) 0.0197(9) Uani 1 1 d . . .
C51 C 0.3712(4) -0.3905(4) 0.2261(3) 0.0181(9) Uani 1 1 d . . .
C61 C 0.2658(4) -0.0207(4) 0.1055(2) 0.0146(8) Uani 1 1 d . . .
C62 C 0.3427(4) -0.0871(4) 0.0432(2) 0.0119(8) Uani 1 1 d . . .
H62A H 0.3770 -0.1767 0.0540 0.014 Uiso 1 1 calc R . .
C63 C 0.3678(4) -0.0197(4) -0.0344(3) 0.0142(8) Uani 1 1 d . . .
C64 C 0.3170(4) 0.1161(4) -0.0509(3) 0.0155(8) Uani 1 1 d . . .
C65 C 0.2432(4) 0.1804(4) 0.0128(3) 0.0165(9) Uani 1 1 d . . .
H65A H 0.2114 0.2696 0.0032 0.020 Uiso 1 1 calc R . .
C66 C 0.2165(4) 0.1116(4) 0.0908(3) 0.0171(9) Uani 1 1 d . . .
H66A H 0.1656 0.1551 0.1327 0.021 Uiso 1 1 calc R . .
C72 C 0.4839(4) -0.2110(4) -0.0892(3) 0.0169(9) Uani 1 1 d . . .
H72A H 0.4081 -0.2320 -0.0697 0.020 Uiso 1 1 calc R . .
H72B H 0.5518 -0.2587 -0.0476 0.020 Uiso 1 1 calc R . .
C73 C 0.5415(4) -0.2472(4) -0.1719(3) 0.0178(9) Uani 1 1 d . . .
H73A H 0.6148 -0.2229 -0.1925 0.021 Uiso 1 1 calc R . .
H73B H 0.5768 -0.3400 -0.1653 0.021 Uiso 1 1 calc R . .
C75 C 0.4744(5) -0.2273(4) -0.3051(3) 0.0291(11) Uani 1 1 d . . .
H75A H 0.4899 -0.3170 -0.2928 0.035 Uiso 1 1 calc R . .
H75B H 0.5572 -0.2222 -0.3306 0.035 Uiso 1 1 calc R . .
C76 C 0.3623(5) -0.1456(4) -0.3644(3) 0.0283(11) Uani 1 1 d . . .
H76A H 0.3703 -0.1917 -0.4066 0.034 Uiso 1 1 calc R . .
H76B H 0.2759 -0.1284 -0.3336 0.034 Uiso 1 1 calc R . .
C78 C 0.2473(4) 0.0622(4) -0.4460(3) 0.0213(10) Uani 1 1 d . . .
H78A H 0.1697 0.0710 -0.4070 0.026 Uiso 1 1 calc R . .
H78B H 0.2395 0.0304 -0.4920 0.026 Uiso 1 1 calc R . .
C79 C 0.2493(5) 0.1908(4) -0.4792(3) 0.0232(10) Uani 1 1 d . . .
H79A H 0.3280 0.1819 -0.5172 0.028 Uiso 1 1 calc R . .
H79B H 0.1692 0.2505 -0.5103 0.028 Uiso 1 1 calc R . .
C81 C 0.2008(5) 0.3764(4) -0.4287(3) 0.0222(10) Uani 1 1 d . . .
H81A H 0.1037 0.4152 -0.4176 0.027 Uiso 1 1 calc R . .
H81B H 0.2201 0.4084 -0.4876 0.027 Uiso 1 1 calc R . .
C82 C 0.2671(5) 0.4112(4) -0.3736(2) 0.0189(9) Uani 1 1 d . . .
H82A H 0.3637 0.3756 -0.3869 0.023 Uiso 1 1 calc R . .
H82B H 0.2317 0.5046 -0.3839 0.023 Uiso 1 1 calc R . .
C84 C 0.3273(4) 0.3643(4) -0.2354(3) 0.0193(9) Uani 1 1 d . . .
H84A H 0.3147 0.4526 -0.2434 0.023 Uiso 1 1 calc R . .
H84B H 0.4209 0.3116 -0.2504 0.023 Uiso 1 1 calc R . .
C85 C 0.2943(4) 0.3140(4) -0.1449(3) 0.0170(9) Uani 1 1 d . . .
H85A H 0.3353 0.3360 -0.1082 0.020 Uiso 1 1 calc R . .
H85B H 0.1973 0.3532 -0.1334 0.020 Uiso 1 1 calc R . .
C202 C 0.2687(7) -0.4243(6) -0.0176(4) 0.0549(17) Uani 1 1 d . . .
H20C H 0.2774 -0.4050 -0.0786 0.066 Uiso 1 1 calc R . .
H20D H 0.3557 -0.4515 0.0041 0.066 Uiso 1 1 calc R . .
C203 C 0.1656(7) -0.3105(6) 0.0127(5) 0.074(2) Uani 1 1 d . . .
H20G H 0.0973 -0.2558 -0.0283 0.088 Uiso 1 1 calc R . .
H20H H 0.2059 -0.2600 0.0240 0.088 Uiso 1 1 calc R . .
C204 C 0.1064(6) -0.3662(6) 0.0916(4) 0.0509(17) Uani 1 1 d . . .
H20A H 0.1563 -0.3841 0.1398 0.061 Uiso 1 1 calc R . .
H20B H 0.0124 -0.3082 0.1014 0.061 Uiso 1 1 calc R . .
C205 C 0.1196(7) -0.4864(6) 0.0751(5) 0.063(2) Uani 1 1 d . . .
H20E H 0.1413 -0.5542 0.1260 0.076 Uiso 1 1 calc R . .
H20F H 0.0355 -0.4727 0.0559 0.076 Uiso 1 1 calc R . .
O201 O 0.2239(4) -0.5222(4) 0.0126(3) 0.0599(13) 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C31 Re1 C41 88.20(18) . . ?
C31 Re1 C51 89.66(18) . . ?
C41 Re1 C51 89.09(17) . . ?
C31 Re1 N21 175.40(15) . . ?
C41 Re1 N21 96.27(16) . . ?
C51 Re1 N21 91.50(15) . . ?
C31 Re1 N11 96.67(15) . . ?
C41 Re1 N11 174.86(16) . . ?
C51 Re1 N11 92.57(14) . . ?
N21 Re1 N11 78.82(12) . . ?
C31 Re1 Cl1 92.51(13) . . ?
C41 Re1 Cl1 93.21(14) . . ?
C51 Re1 Cl1 176.88(12) . . ?
N21 Re1 Cl1 86.16(10) . . ?
N11 Re1 Cl1 84.96(9) . . ?
C63 O71 C72 116.8(3) . . ?
C75 O74 C73 112.8(3) . . ?
C76 O77 C78 110.8(3) . . ?
C81 O80 C79 113.2(3) . . ?
C84 O83 C82 110.6(3) . . ?
C64 O86 C85 116.1(3) . . ?
C12 N1 C22 123.7(3) . . ?
C12 N1 C61 116.4(3) . . ?
C22 N1 C61 115.3(3) . . ?
C12 N11 C16 118.5(3) . . ?
C12 N11 Re1 121.2(3) . . ?
C16 N11 Re1 118.3(3) . . ?
C22 N21 C26 118.3(4) . . ?
C22 N21 Re1 123.2(3) . . ?
C26 N21 Re1 118.3(3) . . ?
N11 C12 C13 120.6(4) . . ?
N11 C12 N1 118.5(4) . . ?
C13 C12 N1 120.9(4) . . ?
C14 C13 C12 119.3(4) . . ?
C13 C14 C15 119.8(4) . . ?
C16 C15 C14 117.9(4) . . ?
N11 C16 C15 122.9(4) . . ?
N21 C22 C23 120.9(4) . . ?
N21 C22 N1 118.6(3) . . ?
C23 C22 N1 120.5(4) . . ?
C24 C23 C22 119.4(4) . . ?
C23 C24 C25 120.5(4) . . ?
C26 C25 C24 117.5(4) . . ?
N21 C26 C25 123.3(4) . . ?
O31 C31 Re1 178.2(4) . . ?
O41 C41 Re1 178.9(4) . . ?
O51 C51 Re1 177.0(4) . . ?
C66 C61 C62 120.6(4) . . ?
C66 C61 N1 121.2(3) . . ?
C62 C61 N1 118.1(3) . . ?
C63 C62 C61 119.9(4) . . ?
O71 C63 C62 124.8(3) . . ?
O71 C63 C64 114.9(3) . . ?
C62 C63 C64 120.3(4) . . ?
O86 C64 C65 124.3(3) . . ?
O86 C64 C63 116.7(3) . . ?
C65 C64 C63 119.0(4) . . ?
C64 C65 C66 120.3(4) . . ?
C61 C66 C65 119.8(4) . . ?
O71 C72 C73 108.1(3) . . ?
O74 C73 C72 108.5(3) . . ?
O74 C75 C76 108.8(4) . . ?
O77 C76 C75 110.1(4) . . ?
O77 C78 C79 109.9(4) . . ?
O80 C79 C78 108.9(4) . . ?
O80 C81 C82 108.0(3) . . ?
O83 C82 C81 109.4(3) . . ?
O83 C84 C85 109.1(3) . . ?
O86 C85 C84 109.0(3) . . ?
O201 C202 C203 105.9(5) . . ?
C202 C203 C204 104.0(5) . . ?
C205 C204 C203 103.1(5) . . ?
O201 C205 C204 107.5(5) . . ?
C205 O201 C202 109.7(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 C31 1.911(4) . ?
Re1 C41 1.911(4) . ?
Re1 C51 1.950(5) . ?
Re1 N21 2.175(3) . ?
Re1 N11 2.179(3) . ?
Re1 Cl1 2.4575(16) . ?
O31 C31 1.159(5) . ?
O41 C41 1.156(5) . ?
O51 C51 1.082(5) . ?
O71 C63 1.375(5) . ?
O71 C72 1.432(4) . ?
O74 C75 1.417(5) . ?
O74 C73 1.418(5) . ?
O77 C76 1.410(5) . ?
O77 C78 1.428(5) . ?
O80 C81 1.424(5) . ?
O80 C79 1.424(5) . ?
O83 C84 1.419(5) . ?
O83 C82 1.427(5) . ?
O86 C64 1.363(5) . ?
O86 C85 1.437(4) . ?
N1 C12 1.411(5) . ?
N1 C22 1.423(5) . ?
N1 C61 1.451(5) . ?
N11 C12 1.349(5) . ?
N11 C16 1.355(5) . ?
N21 C22 1.344(5) . ?
N21 C26 1.362(5) . ?
C12 C13 1.396(6) . ?
C13 C14 1.373(6) . ?
C14 C15 1.387(6) . ?
C15 C16 1.371(6) . ?
C22 C23 1.390(6) . ?
C23 C24 1.368(6) . ?
C24 C25 1.380(6) . ?
C25 C26 1.368(6) . ?
C61 C66 1.375(5) . ?
C61 C62 1.394(5) . ?
C62 C63 1.377(5) . ?
C63 C64 1.410(5) . ?
C64 C65 1.392(6) . ?
C65 C66 1.394(6) . ?
C72 C73 1.495(6) . ?
C75 C76 1.501(6) . ?
C78 C79 1.492(6) . ?
C81 C82 1.506(6) . ?
C84 C85 1.504(6) . ?
C202 O201 1.414(7) . ?
C202 C203 1.468(8) . ?
C203 C204 1.491(9) . ?
C204 C205 1.469(8) . ?
C205 O201 1.407(7) . ?
