#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:00:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179435 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/32/4333281.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_4333281
loop_
_publ_author_name
'Kirgan, Robert'
'Simpson, Megan'
'Moore, Curtis'
'Day, Jeff'
'Bui, Loan'
'Tanner, Clayton'
'Rillema, D. Paul'
_publ_section_title
;
 Synthesis, characterization, photophysical, and computational studies of
 rhenium(I) tricarbonyl complexes containing the derivatives of
 bipyrazine.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6464
_journal_page_last               6472
_journal_paper_doi               10.1021/ic700512j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C13 H10 Cl N4 O3 Re'
_chemical_formula_weight         491.90
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   27.1050(5)
_cell_length_b                   27.1050(5)
_cell_length_c                   11.2195(4)
_cell_measurement_reflns_used    8631
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.93
_cell_volume                     7138.4(3)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38984
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    7.844
_exptl_absorpt_correction_T_max  0.4064
_exptl_absorpt_correction_T_min  0.2896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.652
_refine_diff_density_min         -1.385
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0111P)²+7.8678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0401
_reflns_number_gt                2738
_reflns_number_total             3070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700512jsup3.cif
_cod_data_source_block           rk0019
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4333280--4333282.cif.
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4333281
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
C1 C 0.13868(17) 0.07160(16) 0.7479(3) 0.0242(9) Uani 1 1 d .
C2 C 0.23019(15) 0.08350(15) 0.6338(3) 0.0197(8) Uani 1 1 d .
C3 C 0.15479(15) 0.10632(15) 0.5176(4) 0.0213(9) Uani 1 1 d .
C4 C 0.12724(16) 0.18695(16) 0.7500(3) 0.0217(9) Uani 1 1 d .
H4 H 0.1009 0.1502 0.7743 0.026 Uiso 1 1 calc R
C5 C 0.11571(16) 0.23063(16) 0.7708(3) 0.0217(9) Uani 1 1 d .
C6 C 0.20154(17) 0.29314(16) 0.6892(3) 0.0257(9) Uani 1 1 d .
H6 H 0.2290 0.3304 0.6704 0.031 Uiso 1 1 calc R
C7 C 0.21313(15) 0.25013(15) 0.6643(3) 0.0194(8) Uani 1 1 d .
C8 C 0.26283(15) 0.25773(15) 0.5964(3) 0.0182(8) Uani 1 1 d .
C9 C 0.30362(16) 0.30909(15) 0.5477(3) 0.0210(8) Uani 1 1 d .
H9 H 0.3018 0.3417 0.5655 0.025 Uiso 1 1 calc R
C10 C 0.34708(15) 0.26649(15) 0.4544(3) 0.0202(8) Uani 1 1 d .
C11 C 0.30806(15) 0.21495(15) 0.5068(3) 0.0193(8) Uani 1 1 d .
H11 H 0.3115 0.1830 0.4930 0.023 Uiso 1 1 calc R
C12 C 0.06103(16) 0.21923(17) 0.8268(4) 0.0313(10) Uani 1 1 d .
H12A H 0.0667 0.2269 0.9107 0.047 Uiso 1 1 calc R
H12B H 0.0326 0.1801 0.8146 0.047 Uiso 1 1 calc R
H12C H 0.0486 0.2434 0.7911 0.047 Uiso 1 1 calc R
C13 C 0.39138(16) 0.26959(16) 0.3706(3) 0.0265(9) Uani 1 1 d .
H13A H 0.4112 0.3067 0.3349 0.040 Uiso 1 1 calc R
H13B H 0.3735 0.2413 0.3094 0.040 Uiso 1 1 calc R
H13C H 0.4180 0.2627 0.4136 0.040 Uiso 1 1 calc R
Cl1 Cl 0.25767(4) 0.17498(4) 0.84064(8) 0.0261(2) Uani 1 1 d .
N1 N 0.17525(12) 0.19607(12) 0.6957(2) 0.0171(7) Uani 1 1 d .
N2 N 0.26578(12) 0.21010(11) 0.5765(2) 0.0157(6) Uani 1 1 d .
N3 N 0.15296(14) 0.28413(13) 0.7386(3) 0.0253(8) Uani 1 1 d .
N4 N 0.34533(12) 0.31422(12) 0.4767(3) 0.0214(7) Uani 1 1 d .
O1 O 0.24875(11) 0.05392(11) 0.6196(2) 0.0293(6) Uani 1 1 d .
O2 O 0.12704(12) 0.08985(12) 0.4347(2) 0.0321(7) Uani 1 1 d .
O3 O 0.10223(12) 0.03567(11) 0.8013(3) 0.0371(7) Uani 1 1 d .
Re1 Re 0.199619(6) 0.132840(6) 0.660837(13) 0.01644(6) 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
O3 C1 Re1 178.8(3)
O1 C2 Re1 178.8(3)
O2 C3 Re1 178.2(4)
N1 C4 C5 122.0(3)
N1 C4 H4 119.0
C5 C4 H4 119.0
N3 C5 C4 120.6(3)
N3 C5 C12 118.1(3)
C4 C5 C12 121.2(3)
N3 C6 C7 123.4(4)
N3 C6 H6 118.3
C7 C6 H6 118.3
N1 C7 C6 119.6(3)
N1 C7 C8 115.7(3)
C6 C7 C8 124.5(3)
N2 C8 C9 119.7(3)
N2 C8 C7 116.1(3)
C9 C8 C7 124.1(3)
N4 C9 C8 123.4(3)
N4 C9 H9 118.3
C8 C9 H9 118.3
N4 C10 C11 120.9(3)
N4 C10 C13 118.6(3)
C11 C10 C13 120.6(3)
N2 C11 C10 121.9(3)
N2 C11 H11 119.0
C10 C11 H11 119.0
C5 C12 H12A 109.5
C5 C12 H12B 109.5
H12A C12 H12B 109.5
C5 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C10 C13 H13A 109.5
C10 C13 H13B 109.5
H13A C13 H13B 109.5
C10 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C4 N1 C7 117.3(3)
C4 N1 Re1 126.1(2)
C7 N1 Re1 116.5(2)
C11 N2 C8 117.4(3)
C11 N2 Re1 127.0(2)
C8 N2 Re1 115.7(2)
C6 N3 C5 116.8(3)
C9 N4 C10 116.6(3)
C2 Re1 C1 87.86(15)
C2 Re1 C3 91.12(15)
C1 Re1 C3 89.58(15)
C2 Re1 N1 173.32(13)
C1 Re1 N1 96.98(13)
C3 Re1 N1 93.50(12)
C2 Re1 N2 99.59(13)
C1 Re1 N2 171.92(13)
C3 Re1 N2 93.37(13)
N1 Re1 N2 75.34(10)
C2 Re1 Cl1 93.13(11)
C1 Re1 Cl1 93.33(11)
C3 Re1 Cl1 174.94(11)
N1 Re1 Cl1 82.04(8)
N2 Re1 Cl1 83.22(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O3 1.149(4)
C1 Re1 1.923(4)
C2 O1 1.151(4)
C2 Re1 1.917(4)
C3 O2 1.137(4)
C3 Re1 1.925(4)
C4 N1 1.343(4)
C4 C5 1.387(5)
C4 H4 0.9300
C5 N3 1.338(5)
C5 C12 1.493(5)
C6 N3 1.334(5)
C6 C7 1.379(5)
C6 H6 0.9300
C7 N1 1.349(4)
C7 C8 1.470(5)
C8 N2 1.351(4)
C8 C9 1.386(5)
C9 N4 1.332(5)
C9 H9 0.9300
C10 N4 1.342(4)
C10 C11 1.392(5)
C10 C13 1.494(5)
C11 N2 1.338(4)
C11 H11 0.9300
C12 H12A 0.9600
C12 H12B 0.9600
C12 H12C 0.9600
C13 H13A 0.9600
C13 H13B 0.9600
C13 H13C 0.9600
Cl1 Re1 2.4602(9)
N1 Re1 2.158(3)
N2 Re1 2.177(3)
