#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:56:07 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/81/7238110.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_7238110
loop_
_publ_author_name
'Scudder, Marcia L.'
'Craig, Donald C.'
'Goodwin, Harold A.'
_publ_section_title
;
 Hydrogen bonding influences on the properties of heavily hydrated
 chloride salts of iron(ii) and ruthenium(ii) complexes of
 2,6-bis(pyrazol-3-yl)pyridine, 2,6-bis(1,2,4-triazol-3-yl)pyridine and
 2,2′∶6′,2″-terpyridine
;
_journal_issue                   107
_journal_name_full               CrystEngComm
_journal_page_first              642
_journal_paper_doi               10.1039/b511825e
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         'C18 H14 Fe N14 2+,2(Cl 1-),6(H2 O)'
_chemical_formula_sum            'C18 H26 Cl2 Fe N14 O6'
_chemical_formula_weight         661.2
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.733(2)
_cell_length_b                   11.733(2)
_cell_length_c                   20.664(4)
_cell_measurement_reflns_used    10
_cell_measurement_temperature    294
_cell_measurement_theta_max      12
_cell_measurement_theta_min      11
_cell_volume                     2844.7(9)
_computing_cell_refinement       'CAD4 Version 5.0, 1989'
_computing_data_collection       'CAD4 Version 5.0, 1989'
_computing_data_reduction        'Local program'
_computing_molecular_graphics    'ORTEP-II, (Johnson, 1976)'
_computing_publication_material  'Local programs'
_computing_structure_refinement  'RAELS, (Rae, 1989)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1382
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360.0
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.70
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     97
_refine_ls_number_reflns         927
_refine_ls_R_factor_gt           0.071
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0004F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                927
_reflns_number_total             1251
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b511825e.txt
_cod_data_source_block           DHG74_[Fe(btp)2]Cl2.6H2O
_cod_original_cell_volume        2844.7(7)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7238110
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2-y,z
3 3/4-y,1/4+x,1/4+z
4 1/4+y,1/4-x,1/4+z
5 -x,-y,-z
6 x,1/2+y,-z
7 1/4+y,3/4-x,3/4-z
8 3/4-y,3/4+x,3/4-z
9 1/2+x,1/2+y,1/2+z
10 1/2-x,-y,1/2+z
11 1/4-y,3/4+x,3/4+z
12 3/4+y,3/4-x,3/4+z
13 1/2-x,1/2-y,1/2-z
14 1/2+x,y,1/2-z
15 3/4+y,1/4-x,1/4-z
16 1/4-y,1/4+x,1/4-z
loop_
_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_type_symbol
_atom_site_occupancy
Fe1 0.5000(0) 0.7500(0) 0.6250(0) 0.0630(6) Uani Fe 1.0
N1 0.3984(3) 0.5999(4) 0.5968(2) 0.065(1) Uani N 1.0
N2 0.2970(4) 0.4543(4) 0.5709(2) 0.078(1) Uani N 1.0
N3 0.3260(4) 0.4999(4) 0.5134(2) 0.077(1) Uani N 1.0
N4 0.5000(0) 0.7500(0) 0.5207(2) 0.059(1) Uani N 1.0
C1 0.3380(5) 0.5125(5) 0.6196(2) 0.075(2) Uani C 1.0
C2 0.3882(4) 0.5874(4) 0.5313(2) 0.061(1) Uani C 1.0
C3 0.4435(4) 0.6704(4) 0.4888(2) 0.063(1) Uani C 1.0
C4 0.4393(6) 0.6678(5) 0.4212(2) 0.081(2) Uani C 1.0
C5 0.5000(0) 0.7500(0) 0.3878(3) 0.091(3) Uani C 1.0
Cl1 0.1413(5) 0.2637(4) 0.5220(2) 0.194(2) Uani Cl 0.5
OW1 0.1726(13) 0.2538(11) 0.5787(5) 0.194(2) Uani O 0.5
OW2 0.0363(7) 0.0373(7) 0.5550(4) 0.359(9) Uani O 1.0
HN2 0.2496 0.3840 0.5757 0.078 Uani H 1.0
HC1 0.3260 0.4944 0.6664 0.075 Uani H 1.0
HC4 0.3938 0.6086 0.3978 0.081 Uani H 1.0
HC5 0.5000 0.7500 0.3394 0.091 Uani H 1.0
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 149.3(2) 1_555 1_555 2_665 no
N1 Fe1 N1 94.01(5) 1_555 1_555 7_466 no
N1 Fe1 N1 94.01(5) 1_555 1_555 8_656 no
N1 Fe1 N4 74.7(1) 1_555 1_555 1_555 no
N1 Fe1 N4 105.3(1) 1_555 1_555 7_466 no
N1 Fe1 N1 94.01(5) 2_665 1_555 7_466 no
N1 Fe1 N1 94.01(5) 2_665 1_555 8_656 no
N1 Fe1 N4 74.7(1) 2_665 1_555 1_555 no
N1 Fe1 N4 105.3(1) 2_665 1_555 7_466 no
N1 Fe1 N1 149.3(2) 7_466 1_555 8_656 no
N1 Fe1 N4 105.3(1) 7_466 1_555 1_555 no
N1 Fe1 N4 74.7(1) 7_466 1_555 7_466 no
N1 Fe1 N4 105.3(1) 8_656 1_555 1_555 no
N1 Fe1 N4 74.7(1) 8_656 1_555 7_466 no
N4 Fe1 N4 180.00(0) 1_555 1_555 7_466 no
Fe1 N1 C1 143.9(3) 1_555 1_555 1_555 no
Fe1 N1 C2 113.3(3) 1_555 1_555 1_555 no
C1 N1 C2 102.8(4) 1_555 1_555 1_555 no
N3 N2 C1 112.2(4) 1_555 1_555 1_555 no
N2 N3 C2 101.7(4) 1_555 1_555 1_555 no
Fe1 N4 C3 120.0(3) 1_555 1_555 1_555 no
Fe1 N4 C3 120.0(3) 1_555 1_555 2_665 no
C3 N4 C3 120.0(5) 1_555 1_555 2_665 no
N1 C1 N2 109.0(4) 1_555 1_555 1_555 no
N1 C2 N3 114.3(4) 1_555 1_555 1_555 no
N1 C2 C3 119.0(4) 1_555 1_555 1_555 no
N3 C2 C3 126.7(4) 1_555 1_555 1_555 no
N4 C3 C2 113.1(4) 1_555 1_555 1_555 no
N4 C3 C4 122.2(5) 1_555 1_555 1_555 no
C2 C3 C4 124.7(5) 1_555 1_555 1_555 no
C3 C4 C5 117.7(5) 1_555 1_555 1_555 no
C4 C5 C4 120.1(6) 1_555 1_555 2_665 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.205(4) 1_555 1_555 no
Fe1 N1 2.205(4) 1_555 2_665 no
Fe1 N1 2.205(4) 1_555 7_466 no
Fe1 N1 2.205(4) 1_555 8_656 no
Fe1 N4 2.154(5) 1_555 1_555 no
Fe1 N4 2.154(5) 1_555 7_466 no
N1 C1 1.332(7) 1_555 1_555 no
N1 C2 1.366(6) 1_555 1_555 no
N2 N3 1.345(5) 1_555 1_555 no
N2 C1 1.308(6) 1_555 1_555 no
N3 C2 1.312(6) 1_555 1_555 no
N4 C3 1.322(5) 1_555 1_555 no
N4 C3 1.322(5) 1_555 2_665 no
C2 C3 1.464(7) 1_555 1_555 no
C3 C4 1.397(6) 1_555 1_555 no
C4 C5 1.384(7) 1_555 1_555 no
C5 C4 1.384(7) 1_555 2_665 no
