#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/75/2237512.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_2237512
loop_
_publ_author_name
'Li, Bin'
_publ_section_title
;
 Diaquabis{5-(pyridin-2-yl-κN)-3-[4-(pyridin-4-yl)phenyl]-1H-1,2,4-triazol-1-ido-κN¹}iron(II)
;
_journal_coeditor_code           IS5245
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m168
_journal_paper_doi               10.1107/S1600536813004601
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe (C18 H12 N5)2 (H2 O)2]'
_chemical_formula_moiety         'C36 H28 Fe N10 O2'
_chemical_formula_sum            'C36 H28 Fe N10 O2'
_chemical_formula_weight         688.53
_chemical_name_systematic
Diaquabis{5-(pyridin-2-yl-κN)-3-[4-(pyridin-4-yl)phenyl]-1H-1,2,4-triazol-1-ido-κN¹}iron(II)
_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                 100.9980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.1965(17)
_cell_length_b                   12.0279(16)
_cell_length_c                   9.9006(13)
_cell_measurement_reflns_used    425
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.98
_cell_measurement_theta_min      2.31
_cell_volume                     1542.6(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7711
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.9378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2722
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1200P)²+1.3369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1838
_reflns_number_gt                2214
_reflns_number_total             2722
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            is5245.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237512
_cod_database_fobs_code          2237512
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_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_symmetry_multiplicity
C C1 0.3747(3) 0.2112(3) -0.1244(4) 0.0363(8) Uani d . 1 1
H H1 0.3428 0.1627 -0.1925 0.044 Uiso calc R 1 1
C C2 0.3486(3) 0.3216(3) -0.1351(4) 0.0412(9) Uani d . 1 1
H H2 0.3004 0.3476 -0.2095 0.049 Uiso calc R 1 1
C C3 0.3951(3) 0.3931(3) -0.0334(4) 0.0425(9) Uani d . 1 1
H H3 0.3786 0.4683 -0.0383 0.051 Uiso calc R 1 1
C C4 0.4663(3) 0.3527(3) 0.0757(4) 0.0377(9) Uani d . 1 1
H H4 0.4977 0.4000 0.1455 0.045 Uiso calc R 1 1
C C5 0.4900(2) 0.2410(3) 0.0795(3) 0.0285(7) Uani d . 1 1
C C6 0.5674(2) 0.1872(3) 0.1860(3) 0.0280(7) Uani d . 1 1
C C7 0.6842(3) 0.1449(3) 0.3520(3) 0.0310(8) Uani d . 1 1
C C8 0.7662(3) 0.1451(3) 0.4768(3) 0.0357(8) Uani d . 1 1
C C9 0.7863(3) 0.2334(4) 0.5670(4) 0.0468(10) Uani d . 1 1
H H9 0.7465 0.2976 0.5507 0.056 Uiso calc R 1 1
C C10 0.8648(3) 0.2276(4) 0.6809(4) 0.0512(11) Uani d . 1 1
H H10 0.8764 0.2881 0.7403 0.061 Uiso calc R 1 1
C C11 0.9267(3) 0.1348(4) 0.7094(4) 0.0456(10) Uani d . 1 1
C C12 0.9037(4) 0.0443(4) 0.6214(5) 0.0576(12) Uani d . 1 1
H H12 0.9421 -0.0207 0.6395 0.069 Uiso calc R 1 1
C C13 0.8253(4) 0.0489(3) 0.5086(5) 0.0557(12) Uani d . 1 1
H H13 0.8112 -0.0132 0.4522 0.067 Uiso calc R 1 1
C C14 1.0144(3) 0.1269(4) 0.8279(4) 0.0515(11) Uani d . 1 1
C C15 1.0280(5) 0.1932(7) 0.9391(6) 0.124(3) Uani d . 1 1
H H15 0.9809 0.2496 0.9455 0.149 Uiso calc R 1 1
C C16 1.1133(6) 0.1770(8) 1.0451(6) 0.132(4) Uani d . 1 1
H H16 1.1206 0.2259 1.1191 0.158 Uiso calc R 1 1
C C17 1.1777(5) 0.0489(6) 0.9320(7) 0.0927(19) Uani d . 1 1
H H17 1.2319 0.0018 0.9229 0.111 Uiso calc R 1 1
C C18 1.0973(5) 0.0595(6) 0.8208(6) 0.0885(19) Uani d . 1 1
H H18 1.0993 0.0205 0.7403 0.106 Uiso calc R 1 1
Fe Fe1 0.5000 0.0000 0.0000 0.0319(3) Uani d S 1 2
N N1 0.4444(2) 0.1702(2) -0.0198(3) 0.0300(6) Uani d . 1 1
N N2 0.5878(2) 0.0804(2) 0.1719(3) 0.0335(7) Uani d . 1 1
N N3 0.6647(2) 0.0523(2) 0.2789(3) 0.0371(7) Uani d . 1 1
N N4 0.6261(2) 0.2328(2) 0.2991(3) 0.0307(7) Uani d . 1 1
N N5 1.1827(3) 0.1012(5) 1.0503(4) 0.0787(14) Uani d . 1 1
O O1 0.3849(2) -0.0453(3) 0.1252(3) 0.0406(6) Uani d . 1 1
H H1W 0.374(3) -0.110(4) 0.140(5) 0.063(15) Uiso d D 1 1
H H2W 0.336(4) -0.002(3) 0.136(5) 0.055(15) Uiso d D 1 1
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'
Fe Fe 0.3463 0.8444 '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 C1 C2 . . 122.8(3)
N1 C1 H1 . . 118.6
C2 C1 H1 . . 118.6
C1 C2 C3 . . 118.5(3)
C1 C2 H2 . . 120.7
C3 C2 H2 . . 120.7
C2 C3 C4 . . 119.7(3)
C2 C3 H3 . . 120.1
C4 C3 H3 . . 120.1
C5 C4 C3 . . 118.9(3)
C5 C4 H4 . . 120.6
C3 C4 H4 . . 120.6
N1 C5 C4 . . 121.8(3)
N1 C5 C6 . . 113.3(3)
C4 C5 C6 . . 124.9(3)
N2 C6 N4 . . 112.6(3)
N2 C6 C5 . . 118.6(3)
N4 C6 C5 . . 128.8(3)
N3 C7 N4 . . 114.1(3)
N3 C7 C8 . . 119.4(3)
N4 C7 C8 . . 126.4(3)
C9 C8 C13 . . 117.5(3)
C9 C8 C7 . . 124.1(3)
C13 C8 C7 . . 118.4(3)
C10 C9 C8 . . 120.7(4)
C10 C9 H9 . . 119.6
C8 C9 H9 . . 119.6
C9 C10 C11 . . 122.1(4)
C9 C10 H10 . . 119.0
C11 C10 H10 . . 119.0
C10 C11 C12 . . 117.0(3)
C10 C11 C14 . . 123.7(4)
C12 C11 C14 . . 119.3(4)
C13 C12 C11 . . 121.3(4)
C13 C12 H12 . . 119.4
C11 C12 H12 . . 119.4
C12 C13 C8 . . 121.3(4)
C12 C13 H13 . . 119.4
C8 C13 H13 . . 119.4
C15 C14 C18 . . 114.1(4)
C15 C14 C11 . . 124.8(4)
C18 C14 C11 . . 120.4(4)
C14 C15 C16 . . 119.6(6)
C14 C15 H15 . . 120.2
C16 C15 H15 . . 120.2
N5 C16 C15 . . 126.4(6)
N5 C16 H16 . . 116.8
C15 C16 H16 . . 116.8
N5 C17 C18 . . 124.3(6)
N5 C17 H17 . . 117.8
C18 C17 H17 . . 117.8
C14 C18 C17 . . 120.8(6)
C14 C18 H18 . . 119.6
C17 C18 H18 . . 119.6
N2 Fe1 N2 . 3_655 180.0(2)
N2 Fe1 N1 . 3_655 103.68(10)
N2 Fe1 N1 3_655 3_655 76.32(10)
N2 Fe1 N1 . . 76.32(10)
N2 Fe1 N1 3_655 . 103.68(10)
N1 Fe1 N1 3_655 . 180.00(14)
N2 Fe1 O1 . 3_655 90.52(11)
N2 Fe1 O1 3_655 3_655 89.48(11)
N1 Fe1 O1 3_655 3_655 91.52(11)
N1 Fe1 O1 . 3_655 88.48(11)
N2 Fe1 O1 . . 89.48(11)
N2 Fe1 O1 3_655 . 90.52(11)
N1 Fe1 O1 3_655 . 88.48(11)
N1 Fe1 O1 . . 91.52(11)
O1 Fe1 O1 3_655 . 180.00(19)
C1 N1 C5 . . 118.3(3)
C1 N1 Fe1 . . 125.9(2)
C5 N1 Fe1 . . 115.6(2)
C6 N2 N3 . . 107.2(3)
C6 N2 Fe1 . . 116.1(2)
N3 N2 Fe1 . . 136.7(2)
C7 N3 N2 . . 104.7(3)
C6 N4 C7 . . 101.4(3)
C16 N5 C17 . . 112.8(5)
Fe1 O1 H1W . . 121(3)
Fe1 O1 H2W . . 123(3)
H1W O1 H2W . . 113(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.341(4)
C1 C2 1.371(5)
C1 H1 0.9300
C2 C3 1.376(5)
C2 H2 0.9300
C3 C4 1.378(5)
C3 H3 0.9300
C4 C5 1.378(5)
C4 H4 0.9300
C5 N1 1.352(4)
C5 C6 1.470(4)
C6 N2 1.325(4)
C6 N4 1.350(4)
C7 N3 1.327(4)
C7 N4 1.351(4)
C7 C8 1.479(4)
C8 C9 1.380(5)
C8 C13 1.397(5)
C9 C10 1.380(5)
C9 H9 0.9300
C10 C11 1.381(6)
C10 H10 0.9300
C11 C12 1.391(6)
C11 C14 1.485(5)
C12 C13 1.371(6)
C12 H12 0.9300
C13 H13 0.9300
C14 C15 1.344(7)
C14 C18 1.374(7)
C15 C16 1.398(7)
C15 H15 0.9300
C16 N5 1.287(9)
C16 H16 0.9300
C17 N5 1.320(8)
C17 C18 1.381(7)
C17 H17 0.9300
C18 H18 0.9300
Fe1 N2 2.103(3)
Fe1 N1 2.171(3)
Fe1 O1 2.205(3)
N2 N3 1.363(4)
O1 H1W 0.81(4)
O1 H2W 0.85(5)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1W N4 2_645 0.81(4) 1.99(4) 2.784(4) 168(4)
O1 H2W N5 1_454 0.85(5) 2.39(5) 3.165(6) 152(5)
