#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/68/2216873.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_2216873
loop_
_publ_author_name
'You, Wei'
'Yang, Xue-Yun'
'Yao, Cheng'
'Huang, Wei'
_publ_section_title
;Bis(4'-chloro-2,2':6',2''-terpyridine-κ³N,N',N'')iron(II)
 dinitrate dihydrate
;
_journal_coeditor_code           AT2511
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m79
_journal_page_last               m79
_journal_paper_doi               10.1107/S1600536807062836
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Fe (C15 H10 Cl N3)2] (N O3)2, 2H2 O'
_chemical_formula_moiety         'C30 H20 Cl2 Fe N6, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C30 H24 Cl2 Fe N8 O8'
_chemical_formula_weight         751.32
_chemical_name_systematic
;
Bis(4'-chloro-2,2':6',2''-terpyridine-κ³N,N',N'')iron(II) dinitrate
dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.668(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.049(2)
_cell_length_b                   18.255(3)
_cell_length_c                   10.0741(14)
_cell_measurement_reflns_used    2481
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.008
_cell_measurement_theta_min      2.319
_cell_volume                     3238.5(8)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8547
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.9308
_exptl_absorpt_correction_T_min  0.9223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0635P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                2120
_reflns_number_total             3192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            at2511.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2216873
_cod_database_fobs_code          2216873
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Fe Fe1 1.0000 0.25347(2) 0.2500 0.04349(18) Uani d S 1
C C1 0.89844(14) 0.28704(15) 0.4385(3) 0.0581(7) Uani d . 1
H H1 0.9074 0.3364 0.4250 0.070 Uiso calc R 1
C C2 0.85298(17) 0.26824(18) 0.5259(3) 0.0733(9) Uani d . 1
H H2 0.8330 0.3045 0.5727 0.088 Uiso calc R 1
C C3 0.83702(17) 0.19608(19) 0.5445(3) 0.0737(9) Uani d . 1
H H3 0.8058 0.1829 0.6027 0.088 Uiso calc R 1
C C4 0.86806(14) 0.14357(16) 0.4753(3) 0.0609(7) Uani d . 1
H H4 0.8569 0.0943 0.4844 0.073 Uiso calc R 1
C C5 0.91552(13) 0.16424(13) 0.3929(2) 0.0484(6) Uani d . 1
C C6 0.95684(13) 0.11401(13) 0.3214(2) 0.0490(6) Uani d . 1
C C7 0.95566(15) 0.03835(13) 0.3241(3) 0.0566(7) Uani d . 1
H H7 0.9262 0.0130 0.3739 0.068 Uiso calc R 1
C C8 1.0000 0.00191(19) 0.2500 0.0569(10) Uani d S 1
C C9 0.87358(14) 0.22036(15) 0.0110(3) 0.0552(7) Uani d . 1
H H9 0.8832 0.1710 0.0305 0.066 Uiso calc R 1
C C10 0.81690(16) 0.23907(17) -0.0981(3) 0.0652(8) Uani d . 1
H H10 0.7888 0.2028 -0.1514 0.078 Uiso calc R 1
C C11 0.80185(16) 0.31174(18) -0.1283(3) 0.0674(8) Uani d . 1
H H11 0.7634 0.3251 -0.2019 0.081 Uiso calc R 1
C C12 0.84469(14) 0.36479(15) -0.0478(3) 0.0582(7) Uani d . 1
H H12 0.8358 0.4143 -0.0666 0.070 Uiso calc R 1
C C13 0.90054(12) 0.34274(13) 0.0603(2) 0.0459(6) Uani d . 1
C C14 0.94967(13) 0.39307(13) 0.1540(2) 0.0461(6) Uani d . 1
C C15 0.94826(14) 0.46877(13) 0.1511(3) 0.0554(7) Uani d . 1
H H15 0.9137 0.4941 0.0849 0.066 Uiso calc R 1
C C16 1.0000 0.50551(19) 0.2500 0.0563(9) Uani d S 1
Cl Cl1 1.0000 -0.09281(5) 0.2500 0.0883(4) Uani d S 1
Cl Cl2 1.0000 0.60025(6) 0.2500 0.0908(4) Uani d S 1
H H4A 0.8087(18) 0.0502(17) -0.052(3) 0.069(11) Uiso d . 1
H H4B 0.809(3) 0.036(3) 0.071(5) 0.16(2) Uiso d . 1
N N1 0.93034(11) 0.23672(10) 0.3718(2) 0.0483(5) Uani d . 1
N N2 1.0000 0.15050(14) 0.2500 0.0450(7) Uani d S 1
N N3 0.91592(11) 0.27102(10) 0.0912(2) 0.0462(5) Uani d . 1
N N4 1.0000 0.35651(14) 0.2500 0.0421(6) Uani d S 1
N N5 0.72096(17) 0.05138(16) 0.6869(3) 0.0819(8) Uani d . 1
O O1 0.7680(2) 0.0029(2) 0.7212(3) 0.1692(17) Uani d . 1
O O2 0.6813(2) 0.05091(14) 0.5761(4) 0.1604(16) Uani d . 1
O O3 0.71662(18) 0.09870(17) 0.7664(3) 0.1287(11) Uani d . 1
O O4 0.84123(15) 0.04554(14) 0.0124(3) 0.0804(7) Uani d . 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'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 '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
_geom_angle_publ_flag
N2 Fe1 N4 . . 180.0000(10) y
N2 Fe1 N1 . . 81.04(6) y
N4 Fe1 N1 . . 98.96(6) y
N2 Fe1 N1 . 2_755 81.04(6) ?
N4 Fe1 N1 . 2_755 98.96(6) ?
N1 Fe1 N1 . 2_755 162.09(11) y
N2 Fe1 N3 . . 99.34(6) y
N4 Fe1 N3 . . 80.66(6) y
N1 Fe1 N3 . . 92.75(8) y
N1 Fe1 N3 2_755 . 90.14(8) y
N2 Fe1 N3 . 2_755 99.34(6) ?
N4 Fe1 N3 . 2_755 80.66(6) ?
N1 Fe1 N3 . 2_755 90.14(8) ?
N1 Fe1 N3 2_755 2_755 92.75(8) ?
N3 Fe1 N3 . 2_755 161.33(11) y
N1 C1 C2 . . 122.2(3) ?
N1 C1 H1 . . 118.9 ?
C2 C1 H1 . . 118.9 ?
C3 C2 C1 . . 120.1(3) ?
C3 C2 H2 . . 120.0 ?
C1 C2 H2 . . 120.0 ?
C2 C3 C4 . . 118.7(3) ?
C2 C3 H3 . . 120.6 ?
C4 C3 H3 . . 120.6 ?
C5 C4 C3 . . 119.6(3) ?
C5 C4 H4 . . 120.2 ?
C3 C4 H4 . . 120.2 ?
C4 C5 N1 . . 121.8(2) ?
C4 C5 C6 . . 125.3(2) ?
N1 C5 C6 . . 112.9(2) ?
N2 C6 C7 . . 121.2(2) ?
N2 C6 C5 . . 111.7(2) ?
C7 C6 C5 . . 127.1(2) ?
C8 C7 C6 . . 117.3(3) ?
C8 C7 H7 . . 121.4 ?
C6 C7 H7 . . 121.4 ?
C7 C8 C7 . 2_755 122.3(3) ?
C7 C8 Cl1 . . 118.84(17) ?
C7 C8 Cl1 2_755 . 118.84(17) ?
N3 C9 C10 . . 122.3(3) ?
N3 C9 H9 . . 118.8 ?
C10 C9 H9 . . 118.8 ?
C9 C10 C11 . . 119.6(3) ?
C9 C10 H10 . . 120.2 ?
C11 C10 H10 . . 120.2 ?
C10 C11 C12 . . 119.1(3) ?
C10 C11 H11 . . 120.4 ?
C12 C11 H11 . . 120.4 ?
C13 C12 C11 . . 118.6(3) ?
C13 C12 H12 . . 120.7 ?
C11 C12 H12 . . 120.7 ?
N3 C13 C12 . . 122.8(2) ?
N3 C13 C14 . . 113.0(2) ?
C12 C13 C14 . . 124.2(2) ?
N4 C14 C15 . . 121.1(2) ?
N4 C14 C13 . . 111.6(2) ?
C15 C14 C13 . . 127.3(2) ?
C16 C15 C14 . . 117.6(2) ?
C16 C15 H15 . . 121.2 ?
C14 C15 H15 . . 121.2 ?
C15 C16 C15 . 2_755 121.9(3) ?
C15 C16 Cl2 . . 119.06(16) ?
C15 C16 Cl2 2_755 . 119.06(16) ?
C1 N1 C5 . . 117.6(2) ?
C1 N1 Fe1 . . 127.63(18) ?
C5 N1 Fe1 . . 114.76(16) ?
C6 N2 C6 2_755 . 120.7(3) ?
C6 N2 Fe1 2_755 . 119.65(14) ?
C6 N2 Fe1 . . 119.65(14) ?
C9 N3 C13 . . 117.5(2) ?
C9 N3 Fe1 . . 127.40(18) ?
C13 N3 Fe1 . . 115.06(15) ?
C14 N4 C14 2_755 . 120.7(3) ?
C14 N4 Fe1 2_755 . 119.65(13) ?
C14 N4 Fe1 . . 119.65(13) ?
O2 N5 O3 . . 121.5(4) ?
O2 N5 O1 . . 119.9(3) ?
O3 N5 O1 . . 118.6(3) ?
H4A O4 H4B . . 95(3) ?
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 N2 . 1.880(3) y
Fe1 N4 . 1.881(3) y
Fe1 N1 . 1.964(2) y
Fe1 N1 2_755 1.964(2) y
Fe1 N3 . 1.975(2) y
Fe1 N3 2_755 1.975(2) y
C1 N1 . 1.340(3) ?
C1 C2 . 1.373(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.370(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.374(4) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.370(3) ?
C4 H4 . 0.9300 ?
C5 N1 . 1.375(3) ?
C5 C6 . 1.467(3) ?
C6 N2 . 1.346(3) ?
C6 C7 . 1.382(3) ?
C7 C8 . 1.379(3) ?
C7 H7 . 0.9300 ?
C8 C7 2_755 1.379(3) ?
C8 Cl1 . 1.729(4) ?
C9 N3 . 1.349(3) ?
C9 C10 . 1.371(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.375(4) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.385(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.372(3) ?
C12 H12 . 0.9300 ?
C13 N3 . 1.360(3) ?
C13 C14 . 1.468(3) ?
C14 N4 . 1.349(3) ?
C14 C15 . 1.382(3) ?
C15 C16 . 1.381(3) ?
C15 H15 . 0.9300 ?
C16 C15 2_755 1.381(3) ?
C16 Cl2 . 1.729(4) ?
N2 C6 2_755 1.346(3) ?
N4 C14 2_755 1.349(3) ?
N5 O2 . 1.187(3) ?
N5 O3 . 1.193(3) ?
N5 O1 . 1.223(4) ?
O4 H4A . 0.78(3) ?
O4 H4B . 0.93(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
O4 H4B O1 6 0.93(5) 1.96(5) 2.859(5) 162(4)
O4 H4A O3 1_554 0.78(3) 2.36(3) 3.114(4) 164(3)
O4 H4A O1 1_554 0.78(3) 2.40(3) 3.042(4) 140(3)
