#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313675.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_4313675
loop_
_publ_author_name
'Shih-Sheng Sun'
'Alistair J. Lees'
'Peter Y. Zavalij'
_publ_section_title
;
 Highly Sensitive Luminescent Metal-Complex Receptors for Anions through
 Charge-Assisted Amide Hydrogen Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3445
_journal_page_last               3453
_journal_paper_doi               10.1021/ic0206589
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
;
Re 1+ (C O)3 (C18 H24 N2) (C5 H6 N), (P F6)
;
_chemical_formula_sum            'C26 H30 F6 N3 O3 P Re'
_chemical_formula_weight         777.71
_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                   10.7397(5)
_cell_length_b                   16.6829(9)
_cell_length_c                   18.0705(10)
_cell_measurement_reflns_used    6391
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      49.071
_cell_measurement_theta_min      4.508
_cell_volume                     3237.7(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia,1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'omega 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  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28609
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0.04
_exptl_absorpt_coefficient_mu    3.869
_exptl_absorpt_correction_T_max  0.7338
_exptl_absorpt_correction_T_min  0.4928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .08
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5066
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[σ²(Fo²)+(0.0489P)²], P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                3112
_reflns_number_total             5066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0206589_2.cif
_cod_data_source_block           structure-9
_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               4313675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.702406(18) 0.2500 0.666100(12) 0.04652(9) Uani 1 2 d S . .
C1 C 0.6429(5) 0.2500 0.7655(3) 0.0507(13) Uani 1 2 d S . .
O1 O 0.6079(4) 0.2500 0.8250(2) 0.0677(11) Uani 1 2 d S . .
C2 C 0.8206(4) 0.1695(3) 0.6941(3) 0.0609(11) Uani 1 1 d . . .
O2 O 0.8894(3) 0.1196(2) 0.7101(2) 0.0894(11) Uani 1 1 d . . .
N1A N 0.5532(3) 0.17155(19) 0.63107(18) 0.0502(7) Uani 1 1 d . . .
C1A C 0.4445(3) 0.2058(2) 0.6106(2) 0.0509(9) Uani 1 1 d . . .
C2A C 0.3420(4) 0.1601(3) 0.5936(3) 0.0694(13) Uani 1 1 d . . .
H2A H 0.2687 0.1851 0.5786 0.083 Uiso 1 1 calc R . .
C3A C 0.3466(5) 0.0772(3) 0.5984(3) 0.0862(17) Uani 1 1 d . . .
C4A C 0.4582(5) 0.0429(3) 0.6177(3) 0.0871(16) Uani 1 1 d . . .
H4A H 0.4659 -0.0126 0.6200 0.104 Uiso 1 1 calc R . .
C5A C 0.5585(4) 0.0911(3) 0.6335(3) 0.0636(11) Uani 1 1 d . . .
H5A H 0.6335 0.0670 0.6464 0.076 Uiso 1 1 calc R . .
C6A C 0.2314(6) 0.0229(5) 0.5823(5) 0.127(3) Uani 1 1 d . . .
C7A C 0.1180(6) 0.0699(5) 0.5666(5) 0.168(4) Uani 1 1 d . . .
H7A1 H 0.1296 0.1000 0.5218 0.253 Uiso 1 1 calc R . .
H7A2 H 0.1022 0.1061 0.6068 0.253 Uiso 1 1 calc R . .
H7A3 H 0.0484 0.0343 0.5608 0.253 Uiso 1 1 calc R . .
C8A C 0.2607(7) -0.0332(4) 0.5211(5) 0.133(3) Uani 1 1 d . . .
H8A1 H 0.1922 -0.0694 0.5141 0.199 Uiso 1 1 calc R . .
H8A2 H 0.3342 -0.0632 0.5332 0.199 Uiso 1 1 calc R . .
H8A3 H 0.2746 -0.0034 0.4765 0.199 Uiso 1 1 calc R . .
C9A C 0.2051(10) -0.0273(9) 0.6535(6) 0.209(7) Uani 1 1 d . . .
H9A1 H 0.1344 -0.0614 0.6453 0.313 Uiso 1 1 calc R . .
H9A2 H 0.1881 0.0082 0.6941 0.313 Uiso 1 1 calc R . .
H9A3 H 0.2765 -0.0596 0.6649 0.313 Uiso 1 1 calc R . .
N1B N 0.7678(4) 0.2500 0.5493(3) 0.0530(12) Uani 1 2 d S . .
C1B C 0.6929(5) 0.2500 0.4890(3) 0.0588(15) Uani 1 2 d S . .
H1B H 0.6071 0.2500 0.4964 0.071 Uiso 1 2 calc SR . .
C2B C 0.7358(7) 0.2500 0.4191(4) 0.0690(18) Uani 1 2 d S . .
H2B H 0.6802 0.2500 0.3796 0.083 Uiso 1 2 calc SR . .
C3B C 0.8638(7) 0.2500 0.4057(4) 0.081(2) Uani 1 2 d S . .
C4B C 0.9414(7) 0.2500 0.4656(4) 0.095(3) Uani 1 2 d S . .
H4B H 1.0273 0.2500 0.4592 0.114 Uiso 1 2 calc SR . .
C5B C 0.8912(6) 0.2500 0.5355(3) 0.0728(19) Uani 1 2 d S . .
H5B H 0.9455 0.2500 0.5756 0.087 Uiso 1 2 calc SR . .
N2B N 0.9116(8) 0.2500 0.3361(3) 0.129(3) Uani 1 2 d S . .
H2B1 H 0.9909 0.2500 0.3297 0.154 Uiso 1 2 calc SR . .
H2B2 H 0.8625 0.2500 0.2985 0.154 Uiso 1 2 calc SR . .
P1 P 0.3313(4) 0.1941(4) 0.3724(2) 0.1286(19) Uani 0.50 1 d PD . .
F1 F 0.4186(19) 0.1658(17) 0.3165(7) 0.325(13) Uani 0.50 1 d PD . .
F2 F 0.2414(10) 0.2119(12) 0.4306(6) 0.234(16) Uani 0.50 1 d PD . .
F3 F 0.4219(8) 0.1628(9) 0.4288(5) 0.193(5) Uani 0.50 1 d PD . .
F4 F 0.272(3) 0.1149(11) 0.372(2) 0.433(19) Uani 0.50 1 d PD . .
F5 F 0.2418(11) 0.2185(10) 0.3145(6) 0.203(9) Uani 0.50 1 d PD . .
F6 F 0.403(2) 0.2689(8) 0.376(2) 0.397(16) Uani 0.50 1 d PD . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C1 Re1 C2 88.44(18) . 7_565 ?
C1 Re1 C2 88.44(17) . . ?
C2 Re1 C2 89.0(3) 7_565 . ?
C1 Re1 N1A 91.58(15) . . ?
C2 Re1 N1A 172.71(16) 7_565 . ?
C2 Re1 N1A 98.27(17) . . ?
C1 Re1 N1A 91.58(15) . 7_565 ?
C2 Re1 N1A 98.27(17) 7_565 7_565 ?
C2 Re1 N1A 172.71(16) . 7_565 ?
N1A Re1 N1A 74.44(17) . 7_565 ?
C1 Re1 N1B 178.84(19) . . ?
C2 Re1 N1B 92.38(16) 7_565 . ?
C2 Re1 N1B 92.38(16) . . ?
N1A Re1 N1B 87.50(13) . . ?
N1A Re1 N1B 87.50(13) 7_565 . ?
O1 C1 Re1 179.7(5) . . ?
O2 C2 Re1 178.1(4) . . ?
C5A N1A C1A 117.9(3) . . ?
C5A N1A Re1 124.3(3) . . ?
C1A N1A Re1 117.7(2) . . ?
N1A C1A C2A 121.3(4) . . ?
N1A C1A C1A 115.0(2) . 7_565 ?
C2A C1A C1A 123.7(3) . 7_565 ?
C1A C2A C3A 120.7(5) . . ?
C1A C2A H2A 119.6 . . ?
C3A C2A H2A 119.6 . . ?
C4A C3A C2A 117.5(5) . . ?
C4A C3A C6A 119.8(6) . . ?
C2A C3A C6A 122.6(6) . . ?
C3A C4A C5A 119.6(5) . . ?
C3A C4A H4A 120.2 . . ?
C5A C4A H4A 120.2 . . ?
N1A C5A C4A 123.0(4) . . ?
N1A C5A H5A 118.5 . . ?
C4A C5A H5A 118.5 . . ?
C7A C6A C8A 111.5(7) . . ?
C7A C6A C9A 107.2(7) . . ?
C8A C6A C9A 108.3(9) . . ?
C7A C6A C3A 112.4(6) . . ?
C8A C6A C3A 109.7(5) . . ?
C9A C6A C3A 107.6(7) . . ?
C6A C7A H7A1 109.5 . . ?
C6A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C6A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
C6A C8A H8A1 109.5 . . ?
C6A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C6A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C6A C9A H9A1 109.5 . . ?
C6A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C6A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C5B N1B C1B 115.7(5) . . ?
C5B N1B Re1 119.1(4) . . ?
C1B N1B Re1 125.1(4) . . ?
C2B C1B N1B 123.5(6) . . ?
C2B C1B H1B 118.2 . . ?
N1B C1B H1B 118.2 . . ?
C1B C2B C3B 120.0(6) . . ?
C1B C2B H2B 120.0 . . ?
C3B C2B H2B 120.0 . . ?
N2B C3B C4B 120.2(8) . . ?
N2B C3B C2B 122.2(7) . . ?
C4B C3B C2B 117.6(6) . . ?
C3B C4B C5B 119.3(7) . . ?
C3B C4B H4B 120.4 . . ?
C5B C4B H4B 120.4 . . ?
N1B C5B C4B 123.8(6) . . ?
N1B C5B H5B 118.1 . . ?
C4B C5B H5B 118.1 . . ?
C3B N2B H2B1 120.0 . . ?
C3B N2B H2B2 120.0 . . ?
H2B1 N2B H2B2 120.0 . . ?
F6 P1 F1 75.2(17) 7_565 . ?
F6 P1 F2 110(2) 7_565 . ?
F1 P1 F2 172.8(15) . . ?
F6 P1 F6 19.6(8) 7_565 . ?
F1 P1 F6 88.1(13) . . ?
F2 P1 F6 98.3(17) . . ?
F6 P1 F4 154.5(16) 7_565 . ?
F1 P1 F4 89.4(17) . . ?
F2 P1 F4 83.9(18) . . ?
F6 P1 F4 173.9(14) . . ?
F6 P1 F5 112.0(18) 7_565 . ?
F1 P1 F5 91.0(9) . . ?
F2 P1 F5 91.3(8) . . ?
F6 P1 F5 97.7(13) . . ?
F4 P1 F5 87.9(11) . . ?
F6 P1 F3 71.0(14) 7_565 . ?
F1 P1 F3 86.7(8) . . ?
F2 P1 F3 90.5(6) . . ?
F6 P1 F3 86.0(9) . . ?
F4 P1 F3 88.3(11) . . ?
F5 P1 F3 175.6(10) . . ?
F6 P1 P1 51.2(9) 7_565 7_565 ?
F1 P1 P1 108.9(13) . 7_565 ?
F2 P1 P1 78.3(8) . 7_565 ?
F6 P1 P1 31.6(9) . 7_565 ?
F4 P1 P1 154.1(13) . 7_565 ?
F5 P1 P1 74.0(7) . 7_565 ?
F3 P1 P1 110.3(7) . 7_565 ?
F6 P1 F5 87.1(14) 7_565 7_565 ?
F1 P1 F5 100.4(8) . 7_565 ?
F2 P1 F5 85.0(7) . 7_565 ?
F6 P1 F5 70.0(11) . 7_565 ?
F4 P1 F5 116.0(10) . 7_565 ?
F5 P1 F5 29.7(9) . 7_565 ?
F3 P1 F5 154.5(9) . 7_565 ?
P1 P1 F5 44.3(4) 7_565 7_565 ?
F6 P1 F2 82.0(17) 7_565 7_565 ?
F1 P1 F2 151.2(14) . 7_565 ?
F2 P1 F2 35.9(11) . 7_565 ?
F6 P1 F2 65.7(14) . 7_565 ?
F4 P1 F2 117.8(18) . 7_565 ?
F5 P1 F2 81.4(7) . 7_565 ?
F3 P1 F2 102.4(6) . 7_565 ?
P1 P1 F2 42.3(4) 7_565 7_565 ?
F5 P1 F2 60.7(6) 7_565 7_565 ?
P1 F1 F6 38.4(9) . 7_565 ?
F2 F2 P1 101.7(8) 7_565 . ?
F2 F2 P1 42.3(4) 7_565 7_565 ?
P1 F2 P1 59.4(7) . 7_565 ?
P1 F3 F6 38.3(7) . 7_565 ?
F5 F5 P1 106.0(7) 7_565 . ?
F5 F5 P1 44.3(4) 7_565 7_565 ?
P1 F5 P1 61.8(6) . 7_565 ?
F6 F6 P1 128.8(9) 7_565 7_565 ?
F6 F6 P1 31.6(9) 7_565 . ?
P1 F6 P1 97.2(17) 7_565 . ?
F6 F6 F3 139.2(14) 7_565 7_565 ?
P1 F6 F3 70.8(15) 7_565 7_565 ?
P1 F6 F3 138(3) . 7_565 ?
F6 F6 F1 135.2(17) 7_565 7_565 ?
P1 F6 F1 66.4(14) 7_565 7_565 ?
P1 F6 F1 129(2) . 7_565 ?
F3 F6 F1 83.8(9) 7_565 7_565 ?
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 1.907(6) . ?
Re1 C2 1.916(5) 7_565 ?
Re1 C2 1.916(5) . ?
Re1 N1A 2.164(3) . ?
Re1 N1A 2.164(3) 7_565 ?
Re1 N1B 2.224(5) . ?
C1 O1 1.139(6) . ?
C2 O2 1.149(5) . ?
N1A C5A 1.343(5) . ?
N1A C1A 1.351(4) . ?
C1A C2A 1.374(5) . ?
C1A C1A 1.476(8) 7_565 ?
C2A C3A 1.387(7) . ?
C2A H2A 0.9300 . ?
C3A C4A 1.373(7) . ?
C3A C6A 1.561(8) . ?
C4A C5A 1.375(6) . ?
C4A H4A 0.9300 . ?
C5A H5A 0.9300 . ?
C6A C7A 1.477(10) . ?
C6A C8A 1.483(8) . ?
C6A C9A 1.560(13) . ?
C7A H7A1 0.9600 . ?
C7A H7A2 0.9600 . ?
C7A H7A3 0.9600 . ?
C8A H8A1 0.9600 . ?
C8A H8A2 0.9600 . ?
C8A H8A3 0.9600 . ?
C9A H9A1 0.9600 . ?
C9A H9A2 0.9600 . ?
C9A H9A3 0.9600 . ?
N1B C5B 1.349(7) . ?
N1B C1B 1.355(7) . ?
C1B C2B 1.346(9) . ?
C1B H1B 0.9300 . ?
C2B C3B 1.396(11) . ?
C2B H2B 0.9300 . ?
C3B N2B 1.358(8) . ?
C3B C4B 1.367(10) . ?
C4B C5B 1.372(9) . ?
C4B H4B 0.9300 . ?
C5B H5B 0.9300 . ?
N2B H2B1 0.8600 . ?
N2B H2B2 0.8600 . ?
P1 F6 0.99(2) 7_565 ?
P1 F1 1.456(9) . ?
P1 F2 1.460(8) . ?
P1 F6 1.465(10) . ?
P1 F4 1.469(10) . ?
P1 F5 1.478(8) . ?
P1 F3 1.503(8) . ?
P1 P1 1.865(14) 7_565 ?
P1 F5 2.035(15) 7_565 ?
P1 F2 2.122(18) 7_565 ?
F1 F6 1.54(3) 7_565 ?
F2 F2 1.27(4) 7_565 ?
F2 P1 2.122(18) 7_565 ?
F3 F6 1.50(2) 7_565 ?
F5 F5 1.05(3) 7_565 ?
F5 P1 2.035(15) 7_565 ?
F6 F6 0.63(3) 7_565 ?
F6 P1 0.99(2) 7_565 ?
F6 F3 1.50(2) 7_565 ?
F6 F1 1.54(3) 7_565 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2B C3B N2B H2B1 180.0 . . . . ?
C2A C3A C6A C7A -3.7(10) . . . . ?
C2A C3A C6A C8A 121.0(7) . . . . ?
C2A C3A C6A C9A -121.4(8) . . . . ?
C3A C6A C7A H7A1 64.4 . . . . ?
C3A C6A C8A H8A1 175.4 . . . . ?
C3A C6A C9A H9A1 180.0 . . . . ?
