#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:33:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179383 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/80/4328028.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_4328028
loop_
_publ_author_name
'Margaret A. Goodman'
'Alexander Y. Nazarenko'
'Barbara J. Casavant'
'Zhanjie Li'
'William W. Brennessel'
'Michael J. DeMarco'
'Gen Long'
'M. Scott Goodman'
_publ_section_title
;
 Tris(5-methylpyrazolyl)methane: Synthesis and Properties of Its Iron(II)
 Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1084
_journal_page_last               1093
_journal_paper_doi               10.1021/ic2022038
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C26 H32 Fe N12, 2(Cl O4)'
_chemical_formula_sum            'C26 H32 Cl2 Fe N12 O8'
_chemical_formula_weight         767.39
_chemical_name_systematic
;
  bis(tris(5-methylpyrazolylmethane))iron(II) perchlorate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.1783(10)
_cell_length_b                   11.1783(10)
_cell_length_c                   21.515(4)
_cell_measurement_reflns_used    4084
_cell_measurement_temperature    263.0(2)
_cell_measurement_theta_max      32.11
_cell_measurement_theta_min      2.31
_cell_volume                     2328.2(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      263.0(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, ω scans per 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10556
_diffrn_reflns_theta_full        32.54
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            pink-red
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0479
_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)+(0.0849P)²+2.5340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                1457
_reflns_number_total             1877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2022038_si_002_7.cif
_cod_data_source_block           ra09
_cod_original_cell_volume        2328.2(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4328028
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.0000 0.0000 0.5000 0.03193(19) Uani 1 6 d S
N1 N 0.03181(18) 0.15455(17) 0.55679(7) 0.0386(4) Uani 1 1 d .
N2 N 0.01689(17) 0.12988(16) 0.61956(6) 0.0356(3) Uani 1 1 d .
C1 C 0.0000 0.0000 0.64109(13) 0.0332(6) Uani 1 3 d S
H1A H 0.0000 0.0000 0.6866 0.040 Uiso 1 3 calc SR
C2 C 0.0609(2) 0.2846(2) 0.55096(10) 0.0468(5) Uani 1 1 d .
H2A H 0.0767 0.3309 0.5133 0.056 Uiso 1 1 calc R
C3 C 0.0644(3) 0.3426(2) 0.60890(11) 0.0490(5) Uani 1 1 d .
H3A H 0.0833 0.4322 0.6166 0.059 Uiso 1 1 calc R
C4 C 0.03467(19) 0.2420(2) 0.65194(9) 0.0379(4) Uani 1 1 d .
C5 C 0.0168(3) 0.2419(3) 0.72070(10) 0.0497(5) Uani 1 1 d .
H5A H 0.0408 0.3331 0.7342 0.075 Uiso 1 1 calc R
H5B H 0.0758 0.2143 0.7408 0.075 Uiso 1 1 calc R
H5C H -0.0776 0.1784 0.7313 0.075 Uiso 1 1 calc R
Cl1 Cl 0.3333 0.6667 0.80228(5) 0.0555(3) Uani 1 3 d S
O1 O 0.3333 0.6667 0.7365(2) 0.1178(19) Uani 1 3 d S
O2 O 0.3112(3) 0.7755(3) 0.82129(14) 0.0981(9) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0385(2) 0.0385(2) 0.0187(3) 0.000 0.000 0.01927(12)
N1 0.0500(9) 0.0429(8) 0.0247(6) 0.0045(6) 0.0030(6) 0.0247(7)
N2 0.0451(8) 0.0384(7) 0.0245(6) 0.0001(5) 0.0012(5) 0.0218(7)
C1 0.0385(9) 0.0385(9) 0.0226(11) 0.000 0.000 0.0193(4)
C2 0.0588(12) 0.0448(10) 0.0399(10) 0.0088(8) 0.0053(9) 0.0282(10)
C3 0.0587(13) 0.0412(10) 0.0504(12) -0.0005(9) 0.0055(9) 0.0274(9)
C4 0.0385(9) 0.0407(9) 0.0350(8) -0.0057(7) 0.0000(7) 0.0201(7)
C5 0.0510(11) 0.0550(12) 0.0381(10) -0.0108(8) 0.0035(8) 0.0228(10)
Cl1 0.0568(4) 0.0568(4) 0.0530(5) 0.000 0.000 0.02838(18)
O1 0.148(3) 0.148(3) 0.058(3) 0.000 0.000 0.0739(15)
O2 0.104(2) 0.0770(15) 0.128(2) 0.0048(15) 0.0326(16) 0.0568(15)
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'
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'
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'
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_3
N1 Fe1 N1 180.00(7) 10_556 .
N1 Fe1 N1 86.48(6) 10_556 12_556
N1 Fe1 N1 93.52(6) . 12_556
N1 Fe1 N1 93.52(6) 10_556 2
N1 Fe1 N1 86.48(6) . 2
N1 Fe1 N1 93.52(6) 12_556 2
N1 Fe1 N1 86.48(6) 10_556 11_556
N1 Fe1 N1 93.52(6) . 11_556
N1 Fe1 N1 86.48(6) 12_556 11_556
N1 Fe1 N1 180.0 2 11_556
N1 Fe1 N1 93.52(6) 10_556 3
N1 Fe1 N1 86.48(6) . 3
N1 Fe1 N1 180.00(7) 12_556 3
N1 Fe1 N1 86.48(6) 2 3
N1 Fe1 N1 93.52(6) 11_556 3
C2 N1 N2 104.58(16) . .
C2 N1 Fe1 136.85(14) . .
N2 N1 Fe1 118.51(12) . .
C4 N2 N1 111.86(15) . .
C4 N2 C1 130.42(17) . .
N1 N2 C1 117.37(16) . .
N2 C1 N2 110.21(11) 2 .
N2 C1 N2 110.21(11) 2 3
N2 C1 N2 110.21(11) . 3
N2 C1 H1A 108.7 2 .
N2 C1 H1A 108.7 . .
N2 C1 H1A 108.7 3 .
N1 C2 C3 111.01(18) . .
N1 C2 H2A 124.5 . .
C3 C2 H2A 124.5 . .
C4 C3 C2 106.55(19) . .
C4 C3 H3A 126.7 . .
C2 C3 H3A 126.7 . .
N2 C4 C3 105.99(17) . .
N2 C4 C5 123.35(19) . .
C3 C4 C5 130.6(2) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O1 Cl1 O2 106.78(13) . .
O1 Cl1 O2 106.78(13) . 2_665
O2 Cl1 O2 112.03(12) . 2_665
O1 Cl1 O2 106.78(13) . 3_565
O2 Cl1 O2 112.03(12) . 3_565
O2 Cl1 O2 112.03(12) 2_665 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9974(16) 10_556
Fe1 N1 1.9974(16) .
Fe1 N1 1.9974(16) 12_556
Fe1 N1 1.9974(16) 2
Fe1 N1 1.9974(16) 11_556
Fe1 N1 1.9974(16) 3
N1 C2 1.327(3) .
N1 N2 1.372(2) .
N2 C4 1.359(2) .
N2 C1 1.4436(18) .
C1 N2 1.4436(18) 2
C1 N2 1.4436(18) 3
C1 H1A 0.9800 .
C2 C3 1.397(3) .
C2 H2A 0.9300 .
C3 C4 1.363(3) .
C3 H3A 0.9300 .
C4 C5 1.493(3) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
Cl1 O1 1.416(5) .
Cl1 O2 1.417(2) .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Fe1 N1 C2 -44.9(3) 12_556 .
N1 Fe1 N1 C2 -138.2(3) 2 .
N1 Fe1 N1 C2 41.8(3) 11_556 .
N1 Fe1 N1 C2 135.1(3) 3 .
N1 Fe1 N1 N2 131.70(11) 12_556 .
N1 Fe1 N1 N2 38.39(11) 2 .
N1 Fe1 N1 N2 -141.61(11) 11_556 .
N1 Fe1 N1 N2 -48.30(11) 3 .
C2 N1 N2 C4 0.7(2) . .
Fe1 N1 N2 C4 -176.82(13) . .
C2 N1 N2 C1 -173.11(15) . .
Fe1 N1 N2 C1 9.3(2) . .
C4 N2 C1 N2 120.9(2) . 2
N1 N2 C1 N2 -66.61(18) . 2
C4 N2 C1 N2 -117.2(2) . 3
N1 N2 C1 N2 55.3(2) . 3
N2 N1 C2 C3 -0.1(2) . .
Fe1 N1 C2 C3 176.80(16) . .
N1 C2 C3 C4 -0.6(3) . .
N1 N2 C4 C3 -1.1(2) . .
C1 N2 C4 C3 171.72(18) . .
N1 N2 C4 C5 176.60(18) . .
C1 N2 C4 C5 -10.6(3) . .
C2 C3 C4 N2 1.0(2) . .
C2 C3 C4 C5 -176.5(2) . .
