#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/95/2209513.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2209513
loop_
_publ_author_name
'Heilmann, Julia'
'Lerner, Hans-Wolfram'
'Bolte, Michael'
_publ_section_title
;
 Tris(2,2'-bipyridyl)iron(II) dibromide 4.5-hydrate
;
_journal_coeditor_code           HB2074
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1477
_journal_page_last               m1478
_journal_paper_doi               10.1107/S1600536806020903
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe (C10 H8 N2)3]Br2, 4.5H2 O'
_chemical_formula_moiety         'C30 H24 Fe N6 2+, 2 Br -, 4.5 H2 O'
_chemical_formula_sum            'C30 H33 Br2 Fe N6 O4.5'
_chemical_formula_weight         765.29
_chemical_name_systematic        ?
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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            4
_cell_length_a                   13.1386(12)
_cell_length_b                   13.1386(12)
_cell_length_c                   21.630(3)
_cell_measurement_reflns_used    12085
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      2.6
_cell_volume                     3233.6(6)
_computing_cell_refinement       X-Area
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        X-Area
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al.,  2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE IPDSII two-circle diffractometer'
_diffrn_measurement_method       ω
_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  0.0971
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25866
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.194
_refine_diff_density_min         -1.166
_refine_ls_abs_structure_details 'Flack (1983), 892 Friedel pairs'
_refine_ls_abs_structure_Flack   0.56(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.1008
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1880P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2605
_refine_ls_wR_factor_ref         0.2829
_reflns_number_gt                1569
_reflns_number_total             2071
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2074.cif
_cod_data_source_block           IV
_cod_original_formula_sum        'C30 H33 Br2 Fe N6 O4.50'
_cod_database_code               2209513
_cod_database_fobs_code          2209513
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.3333 0.6667 0.51370(11) 0.0237(6) Uani d S 1 . .
N N1 0.3245(7) 0.5370(8) 0.5638(5) 0.030(2) Uani d . 1 . .
C C2 0.2488(8) 0.4271(8) 0.5411(5) 0.027(2) Uani d . 1 . .
C C3 0.2273(10) 0.3254(9) 0.5734(6) 0.035(3) Uani d . 1 . .
H H3 0.1719 0.2499 0.5581 0.042 Uiso calc R 1 . .
C C4 0.2888(12) 0.3367(11) 0.6284(7) 0.041(3) Uani d . 1 . .
H H4 0.2783 0.2694 0.6503 0.050 Uiso calc R 1 . .
C C5 0.3638(9) 0.4468(10) 0.6493(6) 0.032(3) Uani d . 1 . .
H H5 0.4042 0.4567 0.6872 0.039 Uiso calc R 1 . .
C C6 0.3821(9) 0.5442(10) 0.6165(5) 0.032(2) Uani d . 1 . .
H H6 0.4378 0.6197 0.6316 0.038 Uiso calc R 1 . .
N N11 0.2157(7) 0.5332(8) 0.4630(4) 0.0276(19) Uani d . 1 . .
C C12 0.1896(8) 0.4246(10) 0.4825(5) 0.029(2) Uani d . 1 . .
C C13 0.1150(10) 0.3242(9) 0.4515(6) 0.037(3) Uani d . 1 . .
H H13 0.0960 0.2495 0.4676 0.045 Uiso calc R 1 . .
C C14 0.0669(10) 0.3330(10) 0.3956(6) 0.041(3) Uani d . 1 . .
H H14 0.0165 0.2644 0.3725 0.050 Uiso calc R 1 . .
C C15 0.0931(9) 0.4413(10) 0.3743(6) 0.037(3) Uani d . 1 . .
H H15 0.0645 0.4501 0.3355 0.044 Uiso calc R 1 . .
C C16 0.1657(9) 0.5421(10) 0.4126(7) 0.040(3) Uani d . 1 . .
H H16 0.1775 0.6169 0.4008 0.048 Uiso calc R 1 . .
Br Br1 0.2892(3) 0.8867(2) 0.7500 0.0750(9) Uani d S 1 . .
Br Br2 0.0000 0.0000 0.5000 0.0702(14) Uani d S 1 . .
O O1 0.0000 0.0000 0.3621(5) 0.028(2) Uani d S 1 . .
O O2 0.5290(13) 0.3246(9) 0.7500 0.041(3) Uani d SU 1 . .
O O3 0.3333 0.6667 0.7500 0.072(7) Uani d S 1 . .
O O4 0.264(4) 0.138(4) 0.7500 0.062(14) Uiso d SP 0.39(5) A 1
O O4' 0.369(6) 0.187(6) 0.7500 0.16(2) Uiso d SP 0.61(5) A 2
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 Fe1 N1 . 3_565 92.7(4)
N1 Fe1 N1 . 2_665 92.7(4)
N1 Fe1 N1 3_565 2_665 92.7(4)
N1 Fe1 N11 . 3_565 171.9(3)
N1 Fe1 N11 3_565 3_565 81.8(3)
N1 Fe1 N11 2_665 3_565 93.5(3)
N1 Fe1 N11 . . 81.8(3)
N1 Fe1 N11 3_565 . 93.5(3)
N1 Fe1 N11 2_665 . 171.9(3)
N11 Fe1 N11 3_565 . 92.6(4)
N1 Fe1 N11 . 2_665 93.5(3)
N1 Fe1 N11 3_565 2_665 171.9(3)
N1 Fe1 N11 2_665 2_665 81.8(3)
N11 Fe1 N11 3_565 2_665 92.6(4)
N11 Fe1 N11 . 2_665 92.6(4)
C6 N1 C2 . . 117.7(10)
C6 N1 Fe1 . . 128.1(8)
C2 N1 Fe1 . . 114.3(7)
N1 C2 C3 . . 121.2(10)
N1 C2 C12 . . 115.3(10)
C3 C2 C12 . . 123.5(10)
C4 C3 C2 . . 119.3(10)
C4 C3 H3 . . 120.4
C2 C3 H3 . . 120.4
C5 C4 C3 . . 117.9(11)
C5 C4 H4 . . 121.0
C3 C4 H4 . . 121.0
C4 C5 C6 . . 121.0(11)
C4 C5 H5 . . 119.5
C6 C5 H5 . . 119.5
N1 C6 C5 . . 122.8(10)
N1 C6 H6 . . 118.6
C5 C6 H6 . . 118.6
C16 N11 C12 . . 118.6(10)
C16 N11 Fe1 . . 125.8(7)
C12 N11 Fe1 . . 115.6(7)
N11 C12 C13 . . 123.2(11)
N11 C12 C2 . . 112.9(10)
C13 C12 C2 . . 124.0(10)
C12 C13 C14 . . 118.8(11)
C12 C13 H13 . . 120.6
C14 C13 H13 . . 120.6
C15 C14 C13 . . 119.3(10)
C15 C14 H14 . . 120.3
C13 C14 H14 . . 120.3
C14 C15 C16 . . 117.9(11)
C14 C15 H15 . . 121.0
C16 C15 H15 . . 121.0
N11 C16 C15 . . 121.8(10)
N11 C16 H16 . . 119.1
C15 C16 H16 . . 119.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 . 1.973(9) y
Fe1 N1 3_565 1.973(9) ?
Fe1 N1 2_665 1.973(9) ?
Fe1 N11 3_565 1.989(9) ?
Fe1 N11 . 1.989(10) y
Fe1 N11 2_665 1.989(9) ?
N1 C6 . 1.344(15) ?
N1 C2 . 1.371(13) ?
C2 C3 . 1.405(14) ?
C2 C12 . 1.480(15) ?
C3 C4 . 1.40(2) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.357(18) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.376(16) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
N11 C16 . 1.308(16) ?
N11 C12 . 1.357(14) ?
C12 C13 . 1.363(15) ?
C13 C14 . 1.40(2) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.366(17) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.445(16) ?
C15 H15 . 0.9500 ?
C16 H16 . 0.9500 ?
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_site_symmetry_1
_geom_torsion
N1 Fe1 N1 C6 3_565 -85.8(7)
N1 Fe1 N1 C6 2_665 7.1(9)
N11 Fe1 N1 C6 . -178.9(9)
N11 Fe1 N1 C6 2_665 89.0(9)
N1 Fe1 N1 C2 3_565 93.5(9)
N1 Fe1 N1 C2 2_665 -173.6(7)
N11 Fe1 N1 C2 . 0.4(7)
N11 Fe1 N1 C2 2_665 -91.6(7)
C6 N1 C2 C3 . 3.2(14)
Fe1 N1 C2 C3 . -176.2(8)
C6 N1 C2 C12 . -178.9(8)
Fe1 N1 C2 C12 . 1.7(10)
N1 C2 C3 C4 . -2.9(17)
C12 C2 C3 C4 . 179.3(11)
C2 C3 C4 C5 . 2.4(19)
C3 C4 C5 C6 . -2.3(19)
C2 N1 C6 C5 . -3.1(15)
Fe1 N1 C6 C5 . 176.2(8)
C4 C5 C6 N1 . 2.7(17)
N1 Fe1 N11 C16 . 179.7(9)
N1 Fe1 N11 C16 3_565 87.4(10)
N11 Fe1 N11 C16 3_565 5.5(10)
N11 Fe1 N11 C16 2_665 -87.2(8)
N1 Fe1 N11 C12 . -2.7(7)
N1 Fe1 N11 C12 3_565 -95.0(7)
N11 Fe1 N11 C12 3_565 -176.9(7)
N11 Fe1 N11 C12 2_665 90.4(9)
C16 N11 C12 C13 . 0.9(15)
Fe1 N11 C12 C13 . -176.9(9)
C16 N11 C12 C2 . -178.0(9)
Fe1 N11 C12 C2 . 4.3(10)
N1 C2 C12 N11 . -3.9(11)
C3 C2 C12 N11 . 174.0(10)
N1 C2 C12 C13 . 177.3(10)
C3 C2 C12 C13 . -4.8(15)
N11 C12 C13 C14 . 3.1(17)
C2 C12 C13 C14 . -178.2(10)
C12 C13 C14 C15 . -1.8(18)
C13 C14 C15 C16 . -2.9(17)
C12 N11 C16 C15 . -6.0(16)
Fe1 N11 C16 C15 . 171.6(8)
C14 C15 C16 N11 . 7.1(17)
