#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/55/2015560.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_2015560
loop_
_publ_author_name
'Colin A. Kilner'
'Malcolm A. Halcrow'
_publ_section_title
;
 An unusual example of a linearly coordinated acetone ligand in a
 six-coordinate iron(II) complex
;
_journal_coeditor_code           GG3033
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m437
_journal_page_last               m439
_journal_paper_doi               10.1107/S0108270106028903
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Fe (C19 H25 N5) (C3 H6 O) (H2 O)2] (B F4)2, 2C3 H6 O'
_chemical_formula_moiety         'C22 H35 Fe N5 O3 2+, 2B F4 -, 2C3 H6 O'
_chemical_formula_sum            'C28 H47 B2 F8 Fe N5 O5'
_chemical_formula_weight         763.18
_chemical_name_systematic
;
diaqua(diethyl ether)[2,6-bis(3-tert-butylpyrazol-1-yl)pyridine]iron(II)
bis(tetrafluoroborate) diethyl ether disolvate
;
_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                 126.3230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4575(4)
_cell_length_b                   12.78270(10)
_cell_length_c                   14.5598(4)
_cell_measurement_reflns_used    36356
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.80
_cell_volume                     3667.40(13)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997\\)'
_computing_data_collection       'COLLECT (Nonius, 1999\\)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    'ORTEX (McArdle, 1995\\)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997\\)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997\\)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       'ω and φ'
_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  0.1305
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36356
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the
program SORTAV See R.H. Blessing (1995), Acta Cryst. A51, 33-38
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.680
_refine_ls_extinction_coef       0.0057(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0459
_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)+(0.062P)²+2.6971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                3718
_reflns_number_total             4190
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gg3033.cif
_cod_data_source_block           I
_cod_original_cell_volume        3667.40(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2015560
_cod_database_fobs_code          2015560
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.0000 0.30658(2) 0.2500 0.02901(14) Uani d S 1 . .
N N2 0.0000 0.47179(15) 0.2500 0.0323(4) Uani d S 1 . .
C C3 0.02961(9) 0.52457(13) 0.21176(14) 0.0346(4) Uani d . 1 . .
C C4 0.03140(10) 0.63327(14) 0.20994(17) 0.0431(4) Uani d . 1 . .
H H4 0.0531 0.6695 0.1826 0.052 Uiso calc R 1 . .
C C5 0.0000 0.68583(19) 0.2500 0.0467(7) Uani d S 1 . .
H H5 0.0000 0.7601 0.2500 0.056 Uiso calc SR 1 . .
N N6 0.05990(8) 0.46157(11) 0.17439(13) 0.0355(3) Uani d . 1 . .
N N7 0.06095(7) 0.35412(11) 0.18478(12) 0.0326(3) Uani d . 1 . .
C C8 0.09541(9) 0.31925(14) 0.14600(15) 0.0340(4) Uani d . 1 . .
C C9 0.11584(11) 0.40403(16) 0.11037(18) 0.0455(5) Uani d . 1 . .
H H9 0.1406 0.4002 0.0791 0.055 Uiso calc R 1 . .
C C10 0.09313(11) 0.49174(15) 0.12972(18) 0.0449(5) Uani d . 1 . .
H H10 0.0992 0.5615 0.1149 0.054 Uiso calc R 1 . .
C C11 0.10866(9) 0.20394(14) 0.14358(16) 0.0363(4) Uani d . 1 . .
C C12 0.14913(10) 0.15894(16) 0.26494(17) 0.0437(4) Uani d . 1 . .
H H12A 0.1943 0.1911 0.3115 0.066 Uiso calc R 1 . .
H H12B 0.1538 0.0831 0.2621 0.066 Uiso calc R 1 . .
H H12C 0.1252 0.1739 0.2986 0.066 Uiso calc R 1 . .
C C13 0.04054(9) 0.14670(15) 0.06605(16) 0.0403(4) Uani d . 1 . .
H H13A 0.0136 0.1568 0.0952 0.060 Uiso calc R 1 . .
H H13B 0.0488 0.0718 0.0649 0.060 Uiso calc R 1 . .
H H13C 0.0157 0.1749 -0.0115 0.060 Uiso calc R 1 . .
C C14 0.14970(11) 0.18863(17) 0.0962(2) 0.0484(5) Uani d . 1 . .
H H14A 0.1246 0.2181 0.0191 0.073 Uiso calc R 1 . .
H H14B 0.1572 0.1138 0.0933 0.073 Uiso calc R 1 . .
H H14C 0.1935 0.2242 0.1456 0.073 Uiso calc R 1 . .
O O15 0.08949(7) 0.30274(11) 0.41547(12) 0.0420(3) Uani d . 1 . .
H H15A 0.1007(14) 0.267(2) 0.469(3) 0.063(6) Uiso d . 1 . .
H H15B 0.1146(15) 0.351(2) 0.441(2) 0.063(6) Uiso d . 1 . .
O O16 0.0000 0.14483(13) 0.2500 0.0447(5) Uani d S 1 . .
C C17 0.0000 0.04961(18) 0.2500 0.0322(5) Uani d S 1 . .
C C18 0.05461(11) -0.01097(17) 0.34977(16) 0.0470(5) Uani d . 1 . .
H H18A 0.0818 -0.0469 0.3302 0.071 Uiso calc R 1 . .
H H18B 0.0344 -0.0627 0.3712 0.071 Uiso calc R 1 . .
H H18C 0.0837 0.0366 0.4139 0.071 Uiso calc R 1 . .
B B19A 0.1530(4) 0.1692(5) 0.6886(5) 0.0332(14) Uani d PD 0.65 A 1
F F20A 0.16075(12) 0.27801(15) 0.6986(2) 0.0612(6) Uani d PD 0.65 A 1
F F21A 0.12620(10) 0.14616(16) 0.57387(14) 0.0493(4) Uani d PD 0.65 A 1
F F22A 0.21371(10) 0.1205(2) 0.76035(19) 0.0547(6) Uani d PD 0.65 A 1
F F23A 0.1030(2) 0.1382(4) 0.7047(4) 0.0624(9) Uani d PD 0.65 A 1
B B19B 0.1408(6) 0.1662(10) 0.6793(11) 0.037(4) Uiso d PD 0.35 B 2
F F20B 0.1244(2) 0.2604(3) 0.6267(4) 0.0604(10) Uiso d PD 0.35 B 2
F F21B 0.1284(2) 0.0865(4) 0.6080(4) 0.0618(10) Uiso d PD 0.35 B 2
F F22B 0.2102(4) 0.1638(5) 0.7691(6) 0.086(2) Uiso d PD 0.35 B 2
F F23B 0.1117(4) 0.1530(7) 0.7312(6) 0.056(2) Uiso d PD 0.35 B 2
O O24 0.16066(8) 0.47987(12) 0.46096(14) 0.0504(4) Uani d . 1 . .
C C25 0.20620(10) 0.50368(16) 0.45374(16) 0.0423(4) Uani d . 1 . .
C C26 0.24263(12) 0.4236(2) 0.4346(2) 0.0601(6) Uani d . 1 . .
H H26A 0.2232 0.3544 0.4274 0.090 Uiso calc R 1 . .
H H26B 0.2908 0.4235 0.4992 0.090 Uiso calc R 1 . .
H H26C 0.2379 0.4400 0.3644 0.090 Uiso calc R 1 . .
C C27 0.22717(14) 0.61492(19) 0.4639(2) 0.0624(6) Uani d . 1 . .
H H27A 0.1976 0.6596 0.4717 0.094 Uiso calc R 1 . .
H H27B 0.2235 0.6352 0.3955 0.094 Uiso calc R 1 . .
H H27C 0.2743 0.6231 0.5312 0.094 Uiso calc R 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
N2 Fe1 N7 . . 74.50(4) yes
N2 Fe1 O15 . . 91.35(4) yes
N2 Fe1 O16 . . 180 yes
N7 Fe1 N7 . 2 149.00(7) yes
N7 Fe1 O15 . . 89.41(6) yes
N7 Fe1 O15 . 2 91.31(6) yes
N7 Fe1 O16 . . 105.50(4) yes
O15 Fe1 O15 . 2 177.30(8) yes
O15 Fe1 O16 . . 88.65(4) yes
C3 N2 C3 2 . 119.0(2) ?
C3 N2 Fe1 . . 120.50(10) ?
N2 C3 C4 . . 123.10(18) ?
N2 C3 N6 . . 114.49(15) ?
C4 C3 N6 . . 122.40(17) ?
C5 C4 C3 . . 116.47(19) ?
C5 C4 H4 . . 121.8 ?
C3 C4 H4 . . 121.8 ?
C4 C5 C4 . 2 121.9(2) ?
C4 C5 H5 . . 119.1 ?
C10 N6 N7 . . 110.86(15) ?
C10 N6 C3 . . 128.55(16) ?
N7 N6 C3 . . 120.54(14) ?
C8 N7 N6 . . 105.11(14) ?
C8 N7 Fe1 . . 145.04(12) ?
N6 N7 Fe1 . . 109.72(10) ?
N7 C8 C9 . . 110.31(16) ?
N7 C8 C11 . . 122.06(16) ?
C9 C8 C11 . . 127.62(17) ?
C10 C9 C8 . . 106.30(17) ?
C10 C9 H9 . . 126.8 ?
C8 C9 H9 . . 126.8 ?
C9 C10 N6 . . 107.41(17) ?
C9 C10 H10 . . 126.3 ?
N6 C10 H10 . . 126.3 ?
C8 C11 C14 . . 109.96(16) ?
C8 C11 C13 . . 109.10(15) ?
C14 C11 C13 . . 108.86(15) ?
C8 C11 C12 . . 109.79(15) ?
C14 C11 C12 . . 108.84(17) ?
C13 C11 C12 . . 110.28(16) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C13 H13A . . 109.5 ?
C11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C11 C14 H14A . . 109.5 ?
C11 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C11 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
Fe1 O15 H15A . . 131(2) ?
Fe1 O15 H15B . . 121(2) ?
H15A O15 H15B . . 105(3) ?
C17 O16 Fe1 . . 180 ?
O16 C17 C18 . . 121.51(12) ?
C18 C17 C18 2 . 117.0(2) ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
F22A B19A F20A . . 110.9(5) ?
F22A B19A F21A . . 110.1(4) ?
F20A B19A F21A . . 105.6(4) ?
F22A B19A F23A . . 113.5(5) ?
F20A B19A F23A . . 109.5(5) ?
F21A B19A F23A . . 107.0(5) ?
F23B B19B F21B . . 113.0(10) ?
F23B B19B F20B . . 110.9(10) ?
F21B B19B F20B . . 112.3(10) ?
F23B B19B F22B . . 103.3(10) ?
F21B B19B F22B . . 107.3(9) ?
F20B B19B F22B . . 109.7(9) ?
O24 C25 C26 . . 121.6(2) ?
O24 C25 C27 . . 120.6(2) ?
C26 C25 C27 . . 117.8(2) ?
C25 C26 H26A . . 109.5 ?
C25 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
C25 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
C25 C27 H27A . . 109.5 ?
C25 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
C25 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N2 2.112(2) yes
Fe1 N7 2.2739(15) yes
Fe1 O15 2.0857(14) yes
Fe1 O16 2.0676(17) yes
N2 C3 1.329(2) ?
C3 C4 1.391(2) ?
C3 N6 1.404(2) ?
C4 C5 1.383(2) ?
C4 H4 0.9500 ?
C5 H5 0.9500 ?
N6 C10 1.363(2) ?
N6 N7 1.3803(19) ?
N7 C8 1.338(2) ?
C8 C9 1.414(3) ?
C8 C11 1.514(2) ?
C9 C10 1.353(3) ?
C9 H9 0.9500 ?
C10 H10 0.9500 ?
C11 C14 1.531(3) ?
C11 C13 1.535(2) ?
C11 C12 1.536(3) ?
C12 H12A 0.9800 ?
C12 H12B 0.9800 ?
C12 H12C 0.9800 ?
C13 H13A 0.9800 ?
C13 H13B 0.9800 ?
C13 H13C 0.9800 ?
C14 H14A 0.9800 ?
C14 H14B 0.9800 ?
C14 H14C 0.9800 ?
O15 H15A 0.80(3) ?
O15 H15B 0.79(3) ?
O16 C17 1.217(3) ?
C17 C18 1.482(2) ?
C18 H18A 0.9800 ?
C18 H18B 0.9800 ?
C18 H18C 0.9800 ?
B19A F22A 1.358(6) ?
B19A F20A 1.400(6) ?
B19A F21A 1.418(6) ?
B19A F23A 1.431(8) ?
B19B F23B 1.322(14) ?
B19B F21B 1.355(13) ?
B19B F20B 1.355(13) ?
B19B F22B 1.400(12) ?
O24 C25 1.218(2) ?
C25 C26 1.488(3) ?
C25 C27 1.489(3) ?
C26 H26A 0.9800 ?
C26 H26B 0.9800 ?
C26 H26C 0.9800 ?
C27 H27A 0.9800 ?
C27 H27B 0.9800 ?
C27 H27C 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O15 H15A F21A 0.80(3) 1.99(3) 2.771(3) 164(3)
O15 H15A F20B 0.80(3) 2.01(3) 2.715(5) 147(3)
O15 H15B O24 0.79(3) 1.92(3) 2.689(2) 165(3)
