#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/97/7009744.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_7009744
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                 104.21(3)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   7.739(4)
_cell_length_b                   9.9690(10)
_cell_length_c                   16.321(2)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.29
_cell_measurement_theta_min      2.04
_cell_volume                     1220.6(7)
_computing_cell_refinement       'Enraf-Nonius software'
_computing_data_collection       'Enraf-Nonius software'
_computing_data_reduction        xtal
_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         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3536
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    .688
_exptl_absorpt_correction_T_max  .884
_exptl_absorpt_correction_T_min  .813
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XTAL absorb                 
;
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_F_000             624
_exptl_crystal_size_max          .53
_exptl_crystal_size_mid          .29
_exptl_crystal_size_min          .2
_refine_diff_density_max         .46
_refine_diff_density_min         -.38
_refine_ls_goodness_of_fit_all   1.421
_refine_ls_goodness_of_fit_ref   1.586
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .067
_refine_ls_R_factor_gt           .044
_refine_ls_shift/su_max          .033
_refine_ls_shift/su_mean         .005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .050
_refine_ls_wR_factor_ref         .045
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -13
_reflns_limit_l_max              22
_reflns_limit_l_min              -22
_reflns_number_gt                2354
_reflns_number_observed          2354
_reflns_number_total             3536
_reflns_threshold_expression     'I    > 3.00 sig(I   )'
_cod_data_source_file            b003299i.txt
_cod_data_source_block           fepz3
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C20 H20 Fe1 N14 O6'
_cod_database_code               7009744
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 1.00000 1.00000 .0289(2) Uani ? ? 1.00000 ? ?
N11 .6155(3) .8803(2) .93409(14) .0328(11) Uani ? ? 1.00000 ? ?
N15 .6946(3) .7670(2) .97185(14) .0338(11) Uani ? ? 1.00000 ? ?
N21 .7088(3) .9738(2) 1.09430(14) .0342(11) Uani ? ? 1.00000 ? ?
N25 .7724(3) .8467(2) 1.11133(14) .0343(11) Uani ? ? 1.00000 ? ?
N31 .3969(3) .8405(2) 1.03929(14) .0336(11) Uani ? ? 1.00000 ? ?
N35 .5018(3) .7310(2) 1.06108(14) .0346(11) Uani ? ? 1.00000 ? ?
C1 .6848(4) .7397(3) 1.05755(18) .0352(13) Uani ? ? 1.00000 ? ?
C12 .6521(4) .8826(3) .85834(18) .0382(14) Uani ? ? 1.00000 ? ?
C13 .7561(4) .7721(3) .8491(2) .0456(16) Uani ? ? 1.00000 ? ?
C14 .7822(4) .7006(3) .9218(2) .0398(15) Uani ? ? 1.00000 ? ?
C22 .8171(4) 1.0494(3) 1.1512(2) .0418(15) Uani ? ? 1.00000 ? ?
C23 .9492(4) .9727(3) 1.2031(2) .0471(17) Uani ? ? 1.00000 ? ?
C24 .9159(4) .8445(3) 1.17728(18) .0402(15) Uani ? ? 1.00000 ? ?
C32 .2400(4) .8047(3) 1.0524(2) .0419(15) Uani ? ? 1.00000 ? ?
C33 .2471(5) .6732(3) 1.0829(2) .0489(17) Uani ? ? 1.00000 ? ?
C34 .4151(4) .6292(3) 1.08759(19) .0423(15) Uani ? ? 1.00000 ? ?
N100 .8624(4) .4213(2) 1.17051(17) .0449(14) Uani ? ? 1.00000 ? ?
O101 .9441(4) .5209(2) 1.15297(19) .0787(17) Uani ? ? 1.00000 ? ?
O102 .9293(3) .3534(2) 1.23306(15) .0577(13) Uani ? ? 1.00000 ? ?
O103 .7139(3) .3927(3) 1.12482(16) .0732(16) Uani ? ? 1.00000 ? ?
H1 .745(3) .658(2) 1.0773(15) .024(6) Uiso ? ? 1.00000 ? ?
H12 .596(4) .955(3) .8199(18) .046(8) Uiso ? ? 1.00000 ? ?
H13 .804(4) .747(3) .807(2) .063(10) Uiso ? ? 1.00000 ? ?
H14 .847(3) .619(3) .9433(17) .039(8) Uiso ? ? 1.00000 ? ?
H22 .804(3) 1.138(3) 1.1514(17) .033(7) Uiso ? ? 1.00000 ? ?
H23 1.030(4) 1.004(3) 1.246(2) .061(10) Uiso ? ? 1.00000 ? ?
H24 .967(4) .768(3) 1.1939(19) .055(10) Uiso ? ? 1.00000 ? ?
H32 .146(4) .871(3) 1.0399(18) .047(9) Uiso ? ? 1.00000 ? ?
H33 .157(4) .624(3) 1.096(2) .069(11) Uiso ? ? 1.00000 ? ?
H34 .477(4) .547(3) 1.1030(18) .042(8) 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'
Cl ? 0 0 .132019 .158997 '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
6 0 -6
-6 0 6
0 -8 0
0 8 0
0 0 -14
0 0 14
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 . . . 87.16(9) ?
N11 Fe N31 . . . 87.87(10) ?
N11 Fe N11 . . '3 677' 180.0000 ?
N11 Fe N21 . . '3 677' 92.84(9) ?
N11 Fe N31 . . '3 677' 92.13(10) ?
N21 Fe N31 . . . 87.61(9) ?
N21 Fe N11 . . '3 677' 92.84(9) ?
N21 Fe N21 . . '3 677' 180.0000 ?
N21 Fe N31 . . '3 677' 92.39(9) ?
N31 Fe N11 . . '3 677' 92.13(10) ?
N31 Fe N21 . . '3 677' 92.39(9) ?
N31 Fe N31 . . '3 677' 180.0000 ?
N11 Fe N21 '3 677' . '3 677' 87.16(9) ?
N11 Fe N31 '3 677' . '3 677' 87.87(10) ?
N21 Fe N31 '3 677' . '3 677' 87.61(9) ?
Fe N11 N15 . . . 118.16(18) ?
Fe N11 C12 . . . 136.54(19) ?
N15 N11 C12 . . . 105.1(2) ?
N11 N15 C1 . . . 118.1(2) ?
N11 N15 C14 . . . 111.6(2) ?
C1 N15 C14 . . . 130.1(2) ?
Fe N21 N25 . . . 118.14(15) ?
Fe N21 C22 . . . 137.3(2) ?
N25 N21 C22 . . . 104.6(2) ?
N21 N25 C1 . . . 118.1(2) ?
N21 N25 C24 . . . 111.3(2) ?
C1 N25 C24 . . . 130.5(2) ?
Fe N31 N35 . . . 118.31(18) ?
Fe N31 C32 . . . 137.01(19) ?
N35 N31 C32 . . . 104.7(2) ?
N31 N35 C1 . . . 118.4(2) ?
N31 N35 C34 . . . 112.2(2) ?
C1 N35 C34 . . . 129.4(2) ?
N15 C1 N25 . . . 108.8(2) ?
N15 C1 N35 . . . 109.7(2) ?
N15 C1 H1 . . . 110.5(16) ?
N25 C1 N35 . . . 110.0(2) ?
N25 C1 H1 . . . 108.0(13) ?
N35 C1 H1 . . . 109.9(15) ?
N11 C12 C13 . . . 110.2(3) ?
N11 C12 H12 . . . 116.3(19) ?
C13 C12 H12 . . . 133.3(19) ?
C12 C13 C14 . . . 106.6(3) ?
C12 C13 H13 . . . 131(2) ?
C14 C13 H13 . . . 122(2) ?
N15 C14 C13 . . . 106.4(3) ?
N15 C14 H14 . . . 118.8(18) ?
C13 C14 H14 . . . 134.9(18) ?
N21 C22 C23 . . . 111.1(3) ?
N21 C22 H22 . . . 120.8(15) ?
C23 C22 H22 . . . 128.0(15) ?
C22 C23 C24 . . . 106.0(3) ?
C22 C23 H23 . . . 125(2) ?
C24 C23 H23 . . . 129(2) ?
N25 C24 C23 . . . 107.0(3) ?
N25 C24 H24 . . . 119.3(19) ?
C23 C24 H24 . . . 133.8(19) ?
N31 C32 C33 . . . 110.5(3) ?
N31 C32 H32 . . . 116.6(18) ?
C33 C32 H32 . . . 132.8(18) ?
C32 C33 C34 . . . 106.0(3) ?
C32 C33 H33 . . . 128(2) ?
C34 C33 H33 . . . 126(2) ?
N35 C34 C33 . . . 106.6(3) ?
N35 C34 H34 . . . 118.4(18) ?
C33 C34 H34 . . . 135.0(18) ?
O101 N100 O102 . . . 119.7(3) ?
O101 N100 O103 . . . 119.5(3) ?
O102 N100 O103 . . . 120.8(3) ?
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 . . 1.963(2) ?
Fe N21 . . 1.956(2) ?
Fe N31 . . 1.957(2) ?
Fe N11 . '3 677' 1.963(2) ?
Fe N21 . '3 677' 1.956(2) ?
Fe N31 . '3 677' 1.957(2) ?
N11 N15 . . 1.358(3) ?
N11 C12 . . 1.335(4) ?
N15 C1 . . 1.445(4) ?
N15 C14 . . 1.355(4) ?
N21 N25 . . 1.363(3) ?
N21 C22 . . 1.324(4) ?
N25 C1 . . 1.440(3) ?
N25 C24 . . 1.344(3) ?
N31 N35 . . 1.355(3) ?
N31 C32 . . 1.332(4) ?
N35 C1 . . 1.434(4) ?
N35 C34 . . 1.345(4) ?
C1 H1 . . .96(2) ?
C12 C13 . . 1.394(5) ?
C12 H12 . . .99(3) ?
C13 C14 . . 1.357(5) ?
C13 H13 . . .89(4) ?
C14 H14 . . .97(3) ?
C22 C23 . . 1.386(4) ?
C22 H22 . . .89(3) ?
C23 C24 . . 1.350(5) ?
C23 H23 . . .87(3) ?
C24 H24 . . .87(3) ?
C32 C33 . . 1.399(4) ?
C32 H32 . . .97(3) ?
C33 C34 . . 1.357(5) ?
C33 H33 . . .92(4) ?
C34 H34 . . .96(3) ?
N100 O101 . . 1.248(4) ?
N100 O102 . . 1.228(3) ?
N100 O103 . . 1.240(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(2) . . ?
Fe N15 2.866(2) . '3 677' ?
Fe N25 2.864(2) . '3 677' ?
Fe N25 2.864(2) . . ?
Fe N35 2.860(2) . . ?
Fe N35 2.860(2) . '3 677' ?
Fe C1 3.000(3) . '3 677' ?
Fe C1 3.000(3) . . ?
Fe C12 3.072(3) . '3 677' ?
Fe C12 3.072(3) . . ?
Fe C22 3.063(3) . '3 677' ?
Fe C22 3.063(3) . . ?
Fe C32 3.068(3) . . ?
Fe C32 3.068(3) . '3 677' ?
N11 N21 2.702(3) . . ?
N11 N21 2.839(3) . '3 677' ?
N11 N25 2.869(3) . . ?
N11 N31 2.823(3) . '3 677' ?
N11 N31 2.719(4) . . ?
N11 N35 2.860(3) . . ?
N11 C1 2.404(4) . . ?
N11 C13 2.239(4) . . ?
N11 C14 2.245(4) . . ?
N11 H12 1.98(3) . . ?
N15 N21 2.855(3) . . ?
N15 N25 2.346(3) . . ?
N15 N31 2.881(4) . . ?
N15 N35 2.354(4) . . ?
N15 C12 2.138(4) . . ?
N15 C13 2.171(4) . . ?
N15 H1 1.99(2) . . ?
N15 H14 2.01(3) . . ?
N21 N31 2.708(3) . . ?
N21 N31 2.824(3) . '3 677' ?
N21 N35 2.879(3) . . ?
N21 C1 2.405(3) . . ?
N21 C23 2.234(4) . . ?
N21 C24 2.236(4) . . ?
N21 H22 1.94(3) . . ?
N25 N31 2.856(3) . . ?
N25 N35 2.354(3) . . ?
N25 C22 2.125(4) . . ?
N25 C23 2.165(4) . . ?
N25 H1 1.96(2) . . ?
N25 H24 1.93(3) . . ?
N31 C1 2.395(4) . . ?
N31 C33 2.244(4) . . ?
N31 C34 2.241(4) . . ?
N31 H32 1.97(3) . . ?
N35 C32 2.127(4) . . ?
N35 C33 2.166(5) . . ?
N35 H1 1.98(2) . . ?
N35 H34 1.99(3) . . ?
C1 C14 2.540(5) . . ?
C1 C24 2.529(4) . . ?
C1 C34 2.512(5) . . ?
C12 C14 2.206(4) . . ?
C12 H13 2.10(3) . . ?
C13 H12 2.19(3) . . ?
C13 H14 2.15(3) . . ?
C14 H13 1.98(3) . . ?
C22 C24 2.185(5) . . ?
C22 H23 2.01(3) . . ?
C23 H22 2.06(3) . . ?
C23 H24 2.05(3) . . ?
C24 H23 2.02(3) . . ?
C32 C34 2.201(4) . . ?
C32 H33 2.09(3) . . ?
C33 H32 2.17(3) . . ?
C33 H34 2.14(3) . . ?
C34 H33 2.04(4) . . ?
O101 O102 2.141(4) . . ?
O101 O103 2.149(4) . . ?
O101 H1 2.20(2) . . ?
O101 H33 2.32(4) . '1 655' ?
O102 O103 2.146(3) . . ?
O103 H34 2.35(3) . . ?
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
? ? ? ? ? ? ? ? ? ?
