#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:13:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179744 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/40/7004037.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_7004037
loop_
_publ_author_name
'Herrick, Richard S.'
'Ziegler, Christopher J.'
'Jameson, Donald L.'
'Aquina, Christopher'
'Çetin, Anıl'
'Franklin, Brenton R.'
'Condon, Laura R.'
'Barone, Natalie'
'Lopez, Joseph'
_publ_section_title
;
 Rhenium(i) compounds bound by tripodal ligands of pyridine and
 N-methylimidazole
;
_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              3605
_journal_page_last               3609
_journal_paper_doi               10.1039/b802170h
_journal_year                    2008
_chemical_formula_sum            'C21 H16 Br Cl3 N3 O4 Re'
_chemical_formula_weight         746.83
_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                 104.105(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1458(11)
_cell_length_b                   12.0720(13)
_cell_length_c                   19.771(2)
_cell_measurement_reflns_used    5482
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.58
_cell_volume                     2348.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20469
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    7.251
_exptl_absorpt_correction_T_max  0.4844
_exptl_absorpt_correction_T_min  0.2180
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.573
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0359
_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)+(0.0321P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                4825
_reflns_number_total             5659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802170h.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/c
_cod_database_code               7004037
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
Re1 Re 0.393848(17) 0.449545(14) 0.670363(9) 0.01343(7) Uani 1 1 d . . .
Br1 Br 0.87212(4) 0.90702(4) 0.65082(2) 0.01833(11) Uani 1 1 d . . .
Cl1 Cl 0.89289(11) 0.09325(10) 0.52912(6) 0.0215(2) Uani 1 1 d . . .
Cl2 Cl 0.78290(12) 0.21055(10) 0.40061(6) 0.0248(3) Uani 1 1 d . . .
Cl3 Cl 0.99425(12) 0.31140(10) 0.50927(7) 0.0299(3) Uani 1 1 d . . .
N1 N 0.3002(3) 0.2850(3) 0.66445(18) 0.0141(7) Uani 1 1 d . . .
N2 N 0.5713(3) 0.3532(3) 0.66463(17) 0.0131(7) Uani 1 1 d . . .
N3 N 0.3509(4) 0.4337(3) 0.55758(19) 0.0154(8) Uani 1 1 d . . .
O1 O 0.4795(3) 0.4515(2) 0.83029(17) 0.0220(8) Uani 1 1 d . . .
O2 O 0.1178(3) 0.5540(3) 0.67059(19) 0.0261(8) Uani 1 1 d . . .
O3 O 0.5214(3) 0.6811(3) 0.67617(18) 0.0278(8) Uani 1 1 d . . .
O4 O 0.4281(3) 0.1417(2) 0.53469(15) 0.0176(7) Uani 1 1 d . . .
C1 C 0.4441(5) 0.4506(3) 0.7712(3) 0.0176(10) Uani 1 1 d . . .
C2 C 0.2210(5) 0.5177(4) 0.6710(2) 0.0173(9) Uani 1 1 d . . .
C3 C 0.4750(4) 0.5948(4) 0.6734(2) 0.0179(9) Uani 1 1 d . . .
C4 C 0.2174(4) 0.2600(4) 0.7067(2) 0.0163(9) Uani 1 1 d . . .
H4 H 0.2035 0.3139 0.7393 0.020 Uiso 1 1 calc R . .
C5 C 0.1527(4) 0.1594(4) 0.7041(2) 0.0188(10) Uani 1 1 d . . .
H5 H 0.0942 0.1448 0.7339 0.023 Uiso 1 1 calc R . .
C6 C 0.1737(4) 0.0807(4) 0.6580(2) 0.0169(9) Uani 1 1 d . . .
H6 H 0.1296 0.0109 0.6558 0.020 Uiso 1 1 calc R . .
C7 C 0.2590(4) 0.1026(4) 0.6148(2) 0.0167(9) Uani 1 1 d . . .
H7 H 0.2748 0.0488 0.5826 0.020 Uiso 1 1 calc R . .
C8 C 0.3207(4) 0.2060(4) 0.6200(2) 0.0147(9) Uani 1 1 d . . .
C9 C 0.6932(4) 0.3732(4) 0.7093(2) 0.0189(10) Uani 1 1 d . . .
H9 H 0.7038 0.4400 0.7355 0.023 Uiso 1 1 calc R . .
C10 C 0.8020(5) 0.3031(4) 0.7190(2) 0.0208(10) Uani 1 1 d . . .
H10 H 0.8865 0.3213 0.7500 0.025 Uiso 1 1 calc R . .
C11 C 0.7844(4) 0.2038(4) 0.6818(2) 0.0195(10) Uani 1 1 d . . .
H11 H 0.8562 0.1514 0.6883 0.023 Uiso 1 1 calc R . .
C12 C 0.6616(4) 0.1825(4) 0.6355(2) 0.0173(9) Uani 1 1 d . . .
H12 H 0.6481 0.1148 0.6103 0.021 Uiso 1 1 calc R . .
C13 C 0.5583(4) 0.2600(4) 0.6259(2) 0.0148(9) Uani 1 1 d . . .
C14 C 0.2988(5) 0.5202(4) 0.5157(2) 0.0185(10) Uani 1 1 d . . .
H14 H 0.2976 0.5913 0.5361 0.022 Uiso 1 1 calc R . .
C15 C 0.2479(5) 0.5093(4) 0.4453(2) 0.0234(10) Uani 1 1 d . . .
H15 H 0.2137 0.5719 0.4174 0.028 Uiso 1 1 calc R . .
C16 C 0.2471(5) 0.4069(4) 0.4161(2) 0.0245(11) Uani 1 1 d . . .
H16 H 0.2088 0.3968 0.3676 0.029 Uiso 1 1 calc R . .
C17 C 0.3024(4) 0.3176(4) 0.4574(2) 0.0180(10) Uani 1 1 d . . .
H17 H 0.3024 0.2459 0.4376 0.022 Uiso 1 1 calc R . .
C18 C 0.3574(4) 0.3342(4) 0.5277(2) 0.0143(9) Uani 1 1 d . . .
C19 C 0.4192(4) 0.2363(3) 0.5750(2) 0.0150(9) Uani 1 1 d . . .
C20 C 0.5153(5) 0.1476(4) 0.4869(2) 0.0252(11) Uani 1 1 d . . .
H20A H 0.5603 0.2199 0.4912 0.038 Uiso 1 1 calc R . .
H20B H 0.4607 0.1377 0.4390 0.038 Uiso 1 1 calc R . .
H20C H 0.5840 0.0890 0.4980 0.038 Uiso 1 1 calc R . .
C21 C 0.9311(5) 0.1855(4) 0.4680(2) 0.0225(10) Uani 1 1 d . . .
H21 H 1.0022 0.1516 0.4473 0.027 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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
Cl1 C21 Cl3 110.1(3) . . ?
Cl1 C21 Cl2 109.6(3) . . ?
Cl3 C21 Cl2 110.2(3) . . ?
C13 N2 C9 117.8(4) . . ?
C13 N2 Re1 120.6(3) . . ?
N1 C4 C5 122.3(4) . . ?
N1 C8 C7 123.1(4) . . ?
N1 C8 C19 115.9(4) . . ?
N2 C13 C12 121.3(4) . . ?
N2 C13 C19 118.1(4) . . ?
N2 Re1 N3 82.00(13) . . ?
N2 C9 C10 123.9(4) . . ?
N2 Re1 N1 82.29(13) . . ?
N3 Re1 N1 83.67(13) . . ?
N3 C18 C17 121.3(4) . . ?
N3 C18 C19 118.3(4) . . ?
N3 C14 C15 122.8(4) . . ?
O1 C1 Re1 177.0(4) . . ?
O2 C2 Re1 177.5(4) . . ?
O3 C3 Re1 178.6(4) . . ?
O4 C19 C8 106.0(3) . . ?
O4 C19 C18 110.6(3) . . ?
O4 C19 C13 110.1(3) . . ?
C1 Re1 C2 90.12(18) . . ?
C1 Re1 N2 92.50(16) . . ?
C1 Re1 N1 93.61(15) . . ?
C1 Re1 N3 174.13(16) . . ?
C2 Re1 N1 90.21(16) . . ?
C2 Re1 N2 172.19(16) . . ?
C2 Re1 N3 95.07(16) . . ?
C3 Re1 N3 95.10(16) . . ?
C3 Re1 C1 87.64(18) . . ?
C3 Re1 C2 89.66(18) . . ?
C3 Re1 N2 97.79(16) . . ?
C3 Re1 N1 178.75(16) . . ?
C4 N1 Re1 119.6(3) . . ?
C5 C6 C7 120.0(4) . . ?
C6 C5 C4 119.3(4) . . ?
C6 C7 C8 117.7(4) . . ?
C7 C8 C19 121.1(4) . . ?
C8 N1 C4 117.6(4) . . ?
C8 N1 Re1 122.8(3) . . ?
C8 C19 C18 107.9(3) . . ?
C8 C19 C13 106.6(3) . . ?
C9 C10 C11 117.6(4) . . ?
C9 N2 Re1 120.5(3) . . ?
C11 C12 C13 119.8(4) . . ?
C12 C11 C10 119.3(4) . . ?
C12 C13 C19 120.3(4) . . ?
C13 N2 C9 117.8(4) . . ?
C13 N2 Re1 120.6(3) . . ?
C14 N3 Re1 120.6(3) . . ?
C15 C16 C17 119.8(4) . . ?
C16 C15 C14 118.7(5) . . ?
C17 C18 C19 120.3(4) . . ?
C18 N3 C14 118.1(4) . . ?
C18 N3 Re1 120.6(3) . . ?
C18 C19 C13 115.1(3) . . ?
C18 C17 C16 119.1(4) . . ?
C19 O4 C20 117.7(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 C3 1.932(5) . ?
Re1 C1 1.934(5) . ?
Re1 C2 1.940(5) . ?
Re1 N2 2.169(3) . ?
Re1 N3 2.174(4) . ?
Re1 N1 2.193(4) . ?
Cl1 C21 1.754(5) . ?
Cl2 C21 1.776(5) . ?
Cl3 C21 1.769(5) . ?
N1 C8 1.346(5) . ?
N1 C4 1.355(5) . ?
N2 C13 1.349(5) . ?
N2 C9 1.356(6) . ?
N3 C18 1.348(5) . ?
N3 C14 1.358(5) . ?
O1 C1 1.136(6) . ?
O2 C2 1.132(5) . ?
O3 C3 1.139(5) . ?
O4 C20 1.445(5) . ?
C4 C5 1.375(6) . ?
C6 C5 1.368(6) . ?
C7 C6 1.382(6) . ?
C7 C8 1.390(6) . ?
C10 C9 1.367(6) . ?
C10 C11 1.395(6) . ?
C12 C11 1.378(6) . ?
C13 C12 1.384(6) . ?
C13 C19 1.547(6) . ?
C14 C15 1.366(6) . ?
C16 C15 1.364(7) . ?
C17 C16 1.386(6) . ?
C18 C17 1.381(6) . ?
C18 C19 1.542(6) . ?
C19 O4 1.408(5) . ?
C19 C8 1.536(6) . ?
