#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:01:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179737 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/33/7003329.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_7003329
loop_
_publ_author_name
'Pérez, Julio'
'Riera, Lucía'
'Ion, Laura'
'Riera, Víctor'
'Anderson, Kirsty M.'
'Steed, Jonathan W.'
'Miguel, Daniel'
_publ_section_title
;
 Second-sphere interaction of anions with a weakly binding metal
 complex host: probing the effect of counteranions
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              878
_journal_page_last               886
_journal_paper_doi               10.1039/b715599A
_journal_year                    2008
_chemical_formula_moiety         'C30 H24 N6 O3 Re, Br'
_chemical_formula_sum            'C30 H24 Br N6 O3 Re'
_chemical_formula_weight         782.66
_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                   19.1346(17)
_cell_length_b                   14.3590(13)
_cell_length_c                   10.2350(9)
_cell_measurement_temperature    120(2)
_cell_volume                     2812.1(4)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    X-Seed
_computing_publication_material  X-Seed
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SMART 1k'
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31396
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    5.786
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.780904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.889
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0200
_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)+(0.0126P)²+3.6478P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0412
_reflns_number_gt                3399
_reflns_number_total             3931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715599A.txt
_cod_data_source_block           Compound_8_(Li478)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_sg_symbol_H-M      Pnma
_cod_database_code               7003329
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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 0.004197(6) 0.2500 0.147412(11) 0.01236(4) Uani 1 2 d S . .
Br1 Br -0.036598(16) 0.2500 0.65157(3) 0.02092(7) Uani 1 2 d S . .
O1 O -0.05739(9) 0.10154(12) -0.03382(16) 0.0259(4) Uani 1 1 d . . .
O2 O -0.13046(12) 0.2500 0.3114(2) 0.0267(6) Uani 1 2 d S . .
N1 N 0.05574(9) 0.14173(13) 0.26475(17) 0.0150(4) Uani 1 1 d . . .
N2 N 0.09464(9) 0.05025(13) 0.42161(18) 0.0166(4) Uani 1 1 d . . .
N3 N 0.10333(13) 0.2500 0.0403(2) 0.0155(5) Uani 1 2 d S . .
N4 N 0.18104(13) 0.2500 -0.1181(2) 0.0156(5) Uani 1 2 d S . .
C1 C -0.03502(11) 0.15681(16) 0.0355(2) 0.0171(4) Uani 1 1 d . . .
C2 C -0.07960(16) 0.2500 0.2517(3) 0.0180(6) Uani 1 2 d S . .
C11 C 0.05887(11) 0.12876(16) 0.3928(2) 0.0155(4) Uani 1 1 d . . .
H11 H 0.0387 0.1692 0.4559 0.019 Uiso 1 1 calc R . .
C12 C 0.09024(12) 0.06635(16) 0.2097(2) 0.0202(5) Uani 1 1 d . . .
H12 H 0.0962 0.0561 0.1187 0.024 Uiso 1 1 calc R . .
C13 C 0.11414(13) 0.00971(17) 0.3049(2) 0.0219(5) Uani 1 1 d . . .
H13 H 0.1393 -0.0468 0.2938 0.026 Uiso 1 1 calc R . .
C14 C 0.11550(11) 0.02198(16) 0.5506(2) 0.0180(4) Uani 1 1 d . . .
C15 C 0.18009(12) -0.01976(18) 0.5677(2) 0.0250(5) Uani 1 1 d . . .
H15 H 0.2092 -0.0326 0.4947 0.030 Uiso 1 1 calc R . .
C16 C 0.20168(13) -0.0426(2) 0.6933(3) 0.0304(6) Uani 1 1 d . . .
H16 H 0.2456 -0.0720 0.7063 0.036 Uiso 1 1 calc R . .
C17 C 0.15965(13) -0.02297(19) 0.7991(3) 0.0274(5) Uani 1 1 d . . .
H17 H 0.1750 -0.0379 0.8848 0.033 Uiso 1 1 calc R . .
C18 C 0.09488(13) 0.01859(17) 0.7806(2) 0.0235(5) Uani 1 1 d . . .
H18 H 0.0659 0.0320 0.8537 0.028 Uiso 1 1 calc R . .
C19 C 0.07236(12) 0.04062(16) 0.6551(2) 0.0202(4) Uani 1 1 d . . .
H19 H 0.0278 0.0682 0.6417 0.024 Uiso 1 1 calc R . .
C21 C 0.11250(15) 0.2500 -0.0883(3) 0.0157(6) Uani 1 2 d S . .
H21 H 0.0757 0.2500 -0.1507 0.019 Uiso 1 2 calc SR . .
C22 C 0.16948(17) 0.2500 0.0947(3) 0.0220(7) Uani 1 2 d S . .
H22 H 0.1794 0.2500 0.1857 0.026 Uiso 1 2 calc SR . .
C23 C 0.21787(17) 0.2500 -0.0016(3) 0.0225(7) Uani 1 2 d S . .
H23 H 0.2672 0.2500 0.0086 0.027 Uiso 1 2 calc SR . .
C24 C 0.21111(16) 0.2500 -0.2469(3) 0.0179(6) Uani 1 2 d S . .
C25 C 0.16914(16) 0.2500 -0.3563(3) 0.0211(7) Uani 1 2 d S . .
H25 H 0.1197 0.2500 -0.3477 0.025 Uiso 1 2 calc SR . .
C26 C 0.19985(18) 0.2500 -0.4796(3) 0.0251(7) Uani 1 2 d S . .
H26 H 0.1711 0.2500 -0.5553 0.030 Uiso 1 2 calc SR . .
C27 C 0.27189(18) 0.2500 -0.4931(3) 0.0287(8) Uani 1 2 d S . .
H27 H 0.2926 0.2500 -0.5774 0.034 Uiso 1 2 calc SR . .
C28 C 0.31315(19) 0.2500 -0.3824(4) 0.0343(9) Uani 1 2 d S . .
H28 H 0.3626 0.2500 -0.3912 0.041 Uiso 1 2 calc SR . .
C29 C 0.28375(17) 0.2500 -0.2594(4) 0.0275(8) Uani 1 2 d S . .
H29 H 0.3126 0.2500 -0.1839 0.033 Uiso 1 2 calc SR . .
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'
Br Br -0.2901 2.4595 '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 C1 88.70(13) . 8_565 ?
C1 Re1 C2 90.29(9) . . ?
C1 Re1 C2 90.29(9) 8_565 . ?
C1 Re1 N3 92.31(8) . . ?
C1 Re1 N3 92.31(8) 8_565 . ?
C2 Re1 N3 176.36(11) . . ?
C1 Re1 N1 175.58(8) . 8_565 ?
C1 Re1 N1 90.47(8) 8_565 8_565 ?
C2 Re1 N1 94.06(8) . 8_565 ?
N3 Re1 N1 83.38(6) . 8_565 ?
C1 Re1 N1 90.47(8) . . ?
C1 Re1 N1 175.58(8) 8_565 . ?
C2 Re1 N1 94.06(8) . . ?
N3 Re1 N1 83.38(6) . . ?
N1 Re1 N1 90.02(9) 8_565 . ?
C11 N1 C12 105.69(18) . . ?
C11 N1 Re1 131.31(15) . . ?
C12 N1 Re1 122.92(14) . . ?
C11 N2 C13 107.46(18) . . ?
C11 N2 C14 125.21(19) . . ?
C13 N2 C14 126.90(19) . . ?
C21 N3 C22 106.1(3) . . ?
C21 N3 Re1 127.6(2) . . ?
C22 N3 Re1 126.2(2) . . ?
C21 N4 C23 107.5(3) . . ?
C21 N4 C24 126.7(3) . . ?
C23 N4 C24 125.8(3) . . ?
O1 C1 Re1 178.3(2) . . ?
O2 C2 Re1 178.5(3) . . ?
N1 C11 N2 110.85(19) . . ?
C13 C12 N1 109.8(2) . . ?
C12 C13 N2 106.2(2) . . ?
C19 C14 C15 121.4(2) . . ?
C19 C14 N2 119.5(2) . . ?
C15 C14 N2 119.1(2) . . ?
C14 C15 C16 119.0(2) . . ?
C17 C16 C15 120.3(2) . . ?
C16 C17 C18 120.1(2) . . ?
C17 C18 C19 120.0(2) . . ?
C14 C19 C18 119.2(2) . . ?
N3 C21 N4 110.7(3) . . ?
C23 C22 N3 109.5(3) . . ?
C22 C23 N4 106.2(3) . . ?
C25 C24 C29 120.4(3) . . ?
C25 C24 N4 120.8(3) . . ?
C29 C24 N4 118.8(3) . . ?
C24 C25 C26 119.4(3) . . ?
C27 C26 C25 120.7(3) . . ?
C28 C27 C26 119.2(3) . . ?
C29 C28 C27 121.0(3) . . ?
C28 C29 C24 119.3(3) . . ?
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 1.914(2) . ?
Re1 C1 1.914(2) 8_565 ?
Re1 C2 1.926(3) . ?
Re1 N3 2.191(3) . ?
Re1 N1 2.1981(18) 8_565 ?
Re1 N1 2.1981(18) . ?
O1 C1 1.148(3) . ?
O2 C2 1.149(4) . ?
N1 C11 1.325(3) . ?
N1 C12 1.387(3) . ?
N2 C11 1.351(3) . ?
N2 C13 1.380(3) . ?
N2 C14 1.437(3) . ?
N3 C21 1.328(4) . ?
N3 C22 1.383(4) . ?
N4 C21 1.347(4) . ?
N4 C23 1.385(4) . ?
N4 C24 1.438(4) . ?
C12 C13 1.349(3) . ?
C14 C19 1.378(3) . ?
C14 C15 1.385(3) . ?
C15 C16 1.390(3) . ?
C16 C17 1.378(4) . ?
C17 C18 1.389(3) . ?
C18 C19 1.391(3) . ?
C22 C23 1.353(4) . ?
C24 C25 1.378(4) . ?
C24 C29 1.396(4) . ?
C25 C26 1.392(4) . ?
C26 C27 1.385(5) . ?
C27 C28 1.381(5) . ?
C28 C29 1.379(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C11 H11 Br1 0.95 2.73 3.658(2) 166.9 .
C19 H19 Br1 0.95 2.89 3.659(2) 139.0 .
C21 H21 Br1 0.95 2.95 3.902(3) 179.0 1_554
C25 H25 Br1 0.95 2.99 3.938(3) 174.5 1_554
