#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/97/7009743.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_7009743
loop_
_publ_author_name
'Anderson, Peter A.'
'Astley, Timothy'
'Hitchman, Michael A.'
'Keene, F. Richard'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Skelton, Brian W.'
'Tiekink, Edward R. T.'
'Toftlund, Hans'
'White, Allan H.'
_publ_section_title
;
 Structures and spectra of bis-tripodal iron(II) chelates, [FeL2]2+,
 where L = tris(pyrazol-1-yl)methane,
 tris(pyridin-2-yl)methane, bis(pyrazol-1-yl)(pyridin-2-yl)methane and
 tris(pyridin-2-yl)phosphine oxide. Magnetism and spin crossover in the
 (pz)3CH case
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3505
_journal_paper_doi               10.1039/b003299i
_journal_year                    2000
_chemical_formula_sum            'C20 H20 Fe N14 O6'
_chemical_formula_weight         608.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 101.67(3)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   9.716(3)
_cell_length_b                   7.740(2)
_cell_length_c                   17.280(6)
_cell_measurement_reflns_used    6
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      15.9
_cell_volume                     1272.6(7)
_computing_cell_refinement       'Enraf Nonius software'
_computing_data_collection       'Enraf Nonius software'
_computing_data_reduction        'xtal ADDREF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  xtal
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type
;
 CAD4 diffractometer
;
_diffrn_measurement_method       '2θ-ω scans'
_diffrn_radiation_detector       'single counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_sigmaI/netI    0
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2240
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    .66
_exptl_absorpt_correction_T_max  .901
_exptl_absorpt_correction_T_min  .87
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XTAL absorb               
;
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             624
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .16
_refine_diff_density_max         .51
_refine_diff_density_min         -.45
_refine_ls_goodness_of_fit_all   1.457
_refine_ls_goodness_of_fit_ref   1.69
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     255
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .059
_refine_ls_R_factor_gt           .047
_refine_ls_shift/su_max          .028
_refine_ls_shift/su_mean         .0028
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .058
_refine_ls_wR_factor_ref         .056
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         9.119
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                1786
_reflns_number_total             2240
_reflns_threshold_expression     'I    > 3.00 sig(I   )'
_cod_data_source_file            b003299i.txt
_cod_data_source_block           pz3fen
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_database_code               7009743
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+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_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe .50000 .00000 .00000 .0331(4) Uani ? ? 1.00000 ? ?
N11 .5354(3) -.1495(4) .09454(17) .0395(17) Uani ? ? 1.00000 ? ?
N15 .4209(3) -.2013(4) .12319(18) .0420(17) Uani ? ? 1.00000 ? ?
N21 .3695(3) .1328(4) .05030(18) .0405(17) Uani ? ? 1.00000 ? ?
N25 .2798(3) .0444(4) .08635(18) .0407(17) Uani ? ? 1.00000 ? ?
N31 .3430(3) -.1546(4) -.04314(17) .0389(17) Uani ? ? 1.00000 ? ?
N35 .2526(3) -.2013(4) .00456(18) .0406(17) Uani ? ? 1.00000 ? ?
C1 .2854(4) -.1414(5) .0859(2) .041(2) Uani ? ? 1.00000 ? ?
C12 .6427(5) -.2316(6) .1367(2) .049(2) Uani ? ? 1.00000 ? ?
C13 .5987(6) -.3384(6) .1923(3) .056(3) Uani ? ? 1.00000 ? ?
C14 .4600(5) -.3174(6) .1829(2) .050(2) Uani ? ? 1.00000 ? ?
C22 .3417(5) .2993(6) .0606(3) .052(2) Uani ? ? 1.00000 ? ?
C23 .2341(5) .3134(7) .1026(3) .063(3) Uani ? ? 1.00000 ? ?
C24 .1971(5) .1514(6) .1183(3) .053(3) Uani ? ? 1.00000 ? ?
C32 .2920(5) -.2334(6) -.1114(2) .045(2) Uani ? ? 1.00000 ? ?
C33 .1730(5) -.3279(6) -.1073(3) .055(3) Uani ? ? 1.00000 ? ?
C34 .1516(5) -.3057(6) -.0326(3) .049(2) Uani ? ? 1.00000 ? ?
N100 .5253(4) .7854(6) .7007(3) .057(3) Uani ? ? 1.00000 ? ?
O101 .461(2) .865(3) .7458(13) .094(10) Uani ? ? .50000 ? ?
O102 .5736(18) .8571(18) .6504(8) .139(12) Uani ? ? .50000 ? ?
O103 .523(2) .6348(17) .6975(11) .154(12) Uani ? ? .50000 ? ?
O104 .4971(13) .658(2) .6606(12) .157(14) Uani ? ? .50000 ? ?
O105 .6290(12) .8663(18) .6961(6) .086(6) Uani ? ? .50000 ? ?
O106 .4571(17) .829(4) .7448(14) .102(13) Uani ? ? .50000 ? ?
H1 .215(4) -.194(5) .112(2) .047(11) Uiso ? ? 1.00000 ? ?
H12 .735(5) -.216(5) .127(3) .063(14) Uiso ? ? 1.00000 ? ?
H13 .652(4) -.404(6) .224(2) .052(13) Uiso ? ? 1.00000 ? ?
H14 .391(4) -.366(5) .207(2) .052(12) Uiso ? ? 1.00000 ? ?
H22 .405(4) .394(6) .041(2) .064(13) Uiso ? ? 1.00000 ? ?
H23 .197(5) .407(6) .118(3) .062(14) Uiso ? ? 1.00000 ? ?
H24 .117(4) .104(5) .141(2) .054(12) Uiso ? ? 1.00000 ? ?
H32 .341(4) -.227(5) -.151(2) .052(12) Uiso ? ? 1.00000 ? ?
H33 .120(4) -.390(6) -.144(2) .053(13) Uiso ? ? 1.00000 ? ?
H34 .075(4) -.349(5) -.011(2) .051(12) Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 40 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 12 .007996 .005981 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 40 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Fe ? 0 2 .301025 .844971 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 28 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
8 0 0
-8 0 0
0 6 0
0 -6 0
0 0 22
0 0 -22
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N11 Fe N21 . . . 87.75(13) ?
N11 Fe N31 . . . 87.07(12) ?
N11 Fe N11 . . '3 655' 180.0000 ?
N11 Fe N21 . . '3 655' 92.25(13) ?
N11 Fe N31 . . '3 655' 92.93(12) ?
N21 Fe N31 . . . 88.02(13) ?
N21 Fe N11 . . '3 655' 92.25(13) ?
N21 Fe N21 . . '3 655' 180.0000 ?
N21 Fe N31 . . '3 655' 91.98(13) ?
N31 Fe N11 . . '3 655' 92.93(12) ?
N31 Fe N21 . . '3 655' 91.98(13) ?
N31 Fe N31 . . '3 655' 180.0000 ?
N11 Fe N21 '3 655' . '3 655' 87.75(13) ?
N11 Fe N31 '3 655' . '3 655' 87.07(12) ?
N21 Fe N31 '3 655' . '3 655' 88.02(13) ?
Fe N11 N15 . . . 117.0(2) ?
Fe N11 C12 . . . 137.0(3) ?
N15 N11 C12 . . . 105.7(3) ?
N11 N15 C1 . . . 119.2(3) ?
N11 N15 C14 . . . 110.2(3) ?
C1 N15 C14 . . . 130.5(4) ?
Fe N21 N25 . . . 118.2(2) ?
Fe N21 C22 . . . 136.8(3) ?
N25 N21 C22 . . . 105.1(3) ?
N21 N25 C1 . . . 118.3(3) ?
N21 N25 C24 . . . 111.7(3) ?
C1 N25 C24 . . . 130.0(4) ?
Fe N31 N35 . . . 118.4(2) ?
Fe N31 C32 . . . 137.5(3) ?
N35 N31 C32 . . . 104.1(3) ?
N31 N35 C1 . . . 117.1(3) ?
N31 N35 C34 . . . 111.7(3) ?
C1 N35 C34 . . . 131.0(4) ?
N15 C1 N25 . . . 110.8(3) ?
N15 C1 N35 . . . 109.7(3) ?
N15 C1 H1 . . . 109(2) ?
N25 C1 N35 . . . 108.9(3) ?
N25 C1 H1 . . . 112(2) ?
N35 C1 H1 . . . 106(2) ?
N11 C12 C13 . . . 110.5(4) ?
N11 C12 H12 . . . 121(2) ?
C13 C12 H12 . . . 129(2) ?
C12 C13 C14 . . . 106.6(4) ?
C12 C13 H13 . . . 125(3) ?
C14 C13 H13 . . . 128(3) ?
N15 C14 C13 . . . 107.0(4) ?
N15 C14 H14 . . . 119(2) ?
C13 C14 H14 . . . 134(2) ?
N21 C22 C23 . . . 109.7(4) ?
N21 C22 H22 . . . 119(2) ?
C23 C22 H22 . . . 131(2) ?
C22 C23 C24 . . . 106.9(5) ?
C22 C23 H23 . . . 128(3) ?
C24 C23 H23 . . . 125(3) ?
N25 C24 C23 . . . 106.6(4) ?
N25 C24 H24 . . . 120(2) ?
C23 C24 H24 . . . 132(2) ?
N31 C32 C33 . . . 111.2(4) ?
N31 C32 H32 . . . 119(2) ?
C33 C32 H32 . . . 130(2) ?
C32 C33 C34 . . . 105.8(4) ?
C32 C33 H33 . . . 129(3) ?
C34 C33 H33 . . . 125(3) ?
N35 C34 C33 . . . 107.2(4) ?
N35 C34 H34 . . . 125(2) ?
C33 C34 H34 . . . 128(2) ?
O101 N100 O102 . . . 122.6(14) ?
O101 N100 O103 . . . 120.8(16) ?
O101 N100 O104 . . . 132.4(13) ?
O101 N100 O105 . . . 108.4(13) ?
O101 N100 O106 . . . 12.6(18) ?
O102 N100 O103 . . . 115.6(13) ?
O102 N100 O104 . . . 92.2(12) ?
O102 N100 O105 . . . 42.1(9) ?
O102 N100 O106 . . . 134.5(16) ?
O103 N100 O104 . . . 32.3(13) ?
O103 N100 O105 . . . 121.7(13) ?
O103 N100 O106 . . . 108.3(17) ?
O104 N100 O105 . . . 119.0(11) ?
O104 N100 O106 . . . 121.5(15) ?
O105 N100 O106 . . . 119.4(14) ?
N100 O101 O106 . . . 63(6) ?
N100 O102 O104 . . . 44.0(9) ?
N100 O102 O105 . . . 68.9(13) ?
O104 O102 O105 . . . 100.5(16) ?
N100 O103 O104 . . . 77(2) ?
N100 O103 O106 . . . 35.6(10) ?
O104 O103 O106 . . . 96(2) ?
N100 O104 O102 . . . 43.8(8) ?
N100 O104 O103 . . . 71(2) ?
O102 O104 O103 . . . 104(2) ?
N100 O105 O102 . . . 69.0(14) ?
N100 O106 O101 . . . 104(7) ?
N100 O106 O103 . . . 36.1(10) ?
O101 O106 O103 . . . 140(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe N11 . . 1.975(3) ?
Fe N21 . . 1.966(3) ?
Fe N31 . . 1.963(3) ?
Fe N11 . '3 655' 1.975(3) ?
Fe N21 . '3 655' 1.966(3) ?
Fe N31 . '3 655' 1.963(3) ?
N11 N15 . . 1.366(5) ?
N11 C12 . . 1.309(5) ?
N15 C1 . . 1.422(5) ?
N15 C14 . . 1.363(5) ?
N21 N25 . . 1.355(5) ?
N21 C22 . . 1.336(6) ?
N25 C1 . . 1.439(5) ?
N25 C24 . . 1.347(6) ?
N31 N35 . . 1.370(5) ?
N31 C32 . . 1.331(5) ?
N35 C1 . . 1.452(5) ?
N35 C34 . . 1.332(5) ?
C1 H1 . . .98(4) ?
C12 C13 . . 1.398(7) ?
C12 H12 . . .96(5) ?
C13 C14 . . 1.335(7) ?
C13 H13 . . .84(4) ?
C14 H14 . . .93(4) ?
C22 C23 . . 1.393(8) ?
C22 H22 . . 1.06(4) ?
C23 C24 . . 1.347(7) ?
C23 H23 . . .87(5) ?
C24 H24 . . 1.00(4) ?
C32 C33 . . 1.382(7) ?
C32 H32 . . .92(4) ?
C33 C34 . . 1.359(7) ?
C33 H33 . . .87(4) ?
C34 H34 . . .96(4) ?
N100 O101 . . 1.26(3) ?
N100 O102 . . 1.204(17) ?
N100 O103 . . 1.167(14) ?
N100 O104 . . 1.21(2) ?
N100 O105 . . 1.202(13) ?
N100 O106 . . 1.16(2) ?
O101 O106 . . .28(4) ?
O102 O104 . . 1.74(2) ?
O102 O105 . . .863(17) ?
O103 O104 . . .66(3) ?
O103 O106 . . 1.88(3) ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Fe N15 2.866(3) . . ?
Fe N15 2.866(3) . '3 655' ?
Fe N25 2.866(3) . '3 655' ?
Fe N25 2.866(3) . . ?
Fe N35 2.879(3) . '3 655' ?
Fe N35 2.879(3) . . ?
Fe C1 3.000(4) . . ?
Fe C1 3.000(4) . '3 655' ?
Fe C12 3.064(4) . '3 655' ?
Fe C12 3.064(4) . . ?
Fe C22 3.079(5) . . ?
Fe C22 3.079(5) . '3 655' ?
Fe C32 3.079(4) . . ?
Fe C32 3.079(4) . '3 655' ?
N11 N21 2.841(5) . '3 655' ?
N11 N21 2.731(4) . . ?
N11 N25 2.881(4) . . ?
N11 N31 2.712(4) . . ?
N11 N31 2.855(5) . '3 655' ?
N11 N35 2.899(4) . . ?
N11 C1 2.404(5) . . ?
N11 C13 2.224(5) . . ?
N11 C14 2.238(6) . . ?
N11 H12 1.98(4) . . ?
N15 N21 2.875(5) . . ?
N15 N25 2.356(4) . . ?
N15 N31 2.843(4) . . ?
N15 N35 2.350(4) . . ?
N15 C12 2.133(6) . . ?
N15 C13 2.169(6) . . ?
N15 H1 1.97(4) . . ?
N15 H14 1.99(4) . . ?
N21 N31 2.730(4) . . ?
N21 N31 2.826(5) . '3 655' ?
N21 N35 2.870(4) . . ?
N21 C1 2.398(5) . . ?
N21 C23 2.233(7) . . ?
N21 C24 2.236(6) . . ?
N21 H22 2.07(4) . . ?
N25 N31 2.883(5) . . ?
N25 N35 2.352(4) . . ?
N25 C22 2.136(6) . . ?
N25 C23 2.159(6) . . ?
N25 H1 2.03(4) . . ?
N25 H24 2.05(4) . . ?
N31 C1 2.408(5) . . ?
N31 C33 2.239(5) . . ?
N31 C34 2.236(5) . . ?
N31 H32 1.95(4) . . ?
N35 C32 2.130(6) . . ?
N35 C33 2.165(6) . . ?
N35 H1 1.97(4) . . ?
N35 H34 2.04(4) . . ?
C1 C14 2.529(6) . . ?
C1 C24 2.526(7) . . ?
C1 C34 2.534(6) . . ?
C12 C14 2.192(7) . . ?
C12 H13 2.00(4) . . ?
C13 H12 2.13(5) . . ?
C13 H14 2.09(4) . . ?
C14 H13 1.97(4) . . ?
C22 C24 2.201(7) . . ?
C22 H23 2.05(5) . . ?
C23 H22 2.24(4) . . ?
C23 H24 2.16(4) . . ?
C24 H23 1.98(5) . . ?
C32 C34 2.187(7) . . ?
C32 H33 2.05(4) . . ?
C33 H32 2.09(4) . . ?
C33 H34 2.09(4) . . ?
C34 H33 2.00(4) . . ?
O101 O102 2.16(3) . . ?
O101 O103 2.11(3) . . ?
O101 O104 2.25(3) . . ?
O101 O105 1.99(3) . . ?
O101 H32 2.42(5) . '1 566' ?
O102 O103 2.01(2) . . ?
O102 O106 2.18(3) . . ?
O102 H1 2.07(4) . 4 ?
O102 H23 2.32(5) . '4 565' ?
O103 O105 2.07(2) . . ?
O103 H24 2.36(4) . 4 ?
O104 O105 2.08(2) . . ?
O104 O106 2.06(3) . . ?
O104 H1 2.44(4) . 4 ?
O104 H24 2.40(4) . 4 ?
O105 O106 2.04(2) . . ?
O105 H1 2.25(4) . 4 ?
O105 H23 2.39(5) . '4 565' ?
O106 H32 2.34(5) . '1 566' ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?
