#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179312 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/09/4320900.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_4320900
loop_
_publ_author_name
'Yan Z. Voloshin'
'Oleg A. Varzatskii'
'Tatyana E. Kron'
'Vitaly K. Belsky'
'Valery E. Zavodnik'
'Nataly G. Strizhakova'
'Alexey V. Palchik'
_publ_contact_author             'Yan Z. Voloshin'
_publ_contact_author_email       voloshin@cc.nifhi.ac.ru
_publ_section_title
;
 Triribbed-Functionalized Clathrochelate Iron(II) Dioximates as a New and
 Promising Tool To Obtain Polynucleating and Polynuclear Compounds with
 Improved Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1907
_journal_page_last               1918
_journal_paper_doi               10.1021/ic990476n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C14 H16 B2 Cl6 F2 Fe N6 O8'
_chemical_formula_weight         724.52
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.634(4)
_cell_length_b                   8.197(2)
_cell_length_c                   18.799(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      12
_cell_volume                     2714.5(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            1636
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_time  100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.208
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0034(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.116
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_obs          0.0639
_refine_ls_shift/esd_max         0.562
_refine_ls_shift/esd_mean        0.059
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1156P)²+12.5216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1738
_refine_ls_wR_factor_obs         0.1738
_reflns_number_observed          1582
_reflns_number_total             1582
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990476n_4.cif
_cod_data_source_block           yv22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1156P)^2^+12.5216P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1156P)^2^+12.5216P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2715.(1)
_cod_database_code               4320900
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_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.5000 0.80424(15) 0.2500 0.0313(5) Uani 1 d S .
Cl1 Cl 0.59155(11) 1.0358(3) 0.44606(8) 0.0691(7) Uani 1 d . .
Cl2 Cl 0.28727(9) 1.0499(3) 0.18238(10) 0.0735(7) Uani 1 d . .
Cl3 Cl 0.43347(13) 0.3069(3) 0.30909(11) 0.0744(7) Uani 1 d . .
F F 0.3373(2) 0.8038(5) 0.4163(2) 0.0595(12) Uani 1 d . .
O1 O 0.4615(3) 0.8502(7) 0.3964(2) 0.070(2) Uani 1 d . .
O2 O 0.3615(3) 0.9216(8) 0.3097(2) 0.073(2) Uani 1 d . .
O3 O 0.3890(3) 0.6398(7) 0.3335(3) 0.068(2) Uani 1 d . .
N1 N 0.5148(3) 0.8704(8) 0.3466(2) 0.0510(15) Uani 1 d . .
N2 N 0.4051(3) 0.9174(8) 0.2516(3) 0.052(2) Uani 1 d . .
N3 N 0.4458(3) 0.6223(8) 0.2863(3) 0.049(2) Uani 1 d . .
B B 0.3874(4) 0.8040(10) 0.3642(3) 0.043(2) Uani 1 d . .
C1 C 0.5741(3) 0.9530(8) 0.3645(3) 0.044(2) Uani 1 d . .
C2 C 0.3757(3) 0.9707(8) 0.1923(3) 0.045(2) Uani 1 d . .
C3 C 0.4693(4) 0.4796(10) 0.2737(3) 0.046(2) Uani 1 d . .
O4 O 0.3970(11) 0.5034(47) 0.1245(9) 0.137(13) Uani 0.50 d P .
O4A O 0.3907(24) 0.5417(68) 0.1226(23) 0.259(25) Uani 0.50 d P .
C4 C 0.4148(11) 0.5166(24) 0.0508(9) 0.158(6) Uani 1 d . .
C5 C 0.3153(21) 0.5231(50) 0.0255(15) 0.125(12) Uani 0.50 d P .
C6 C 0.2868(9) 0.6073(26) 0.0685(11) 0.162(6) Uani 1 d . .
C7 C 0.3205(7) 0.5263(22) 0.1318(8) 0.141(6) Uani 1 d . .
C5A C 0.3602(23) 0.5766(43) 0.0051(15) 0.113(10) Uani 0.50 d P .
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'
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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
N1 Fe N1 146.9(4) 2_655 . ?
N1 Fe N3 120.9(2) 2_655 . ?
N1 Fe N3 86.0(2) . . ?
N1 Fe N3 86.0(2) 2_655 2_655 ?
N1 Fe N3 120.9(2) . 2_655 ?
N3 Fe N3 77.6(4) . 2_655 ?
N1 Fe N2 86.0(2) 2_655 2_655 ?
N1 Fe N2 78.1(2) . 2_655 ?
N3 Fe N2 146.5(2) . 2_655 ?
N3 Fe N2 85.5(3) 2_655 2_655 ?
N1 Fe N2 78.1(2) 2_655 . ?
N1 Fe N2 85.9(2) . . ?
N3 Fe N2 85.5(3) . . ?
N3 Fe N2 146.5(3) 2_655 . ?
N2 Fe N2 122.0(4) 2_655 . ?
N1 O1 B 112.1(4) . . ?
N2 O2 B 112.0(5) . . ?
N3 O3 B 112.1(5) . . ?
C1 N1 O1 117.6(5) . . ?
C1 N1 Fe 118.6(4) . . ?
O1 N1 Fe 123.4(4) . . ?
C2 N2 O2 117.8(5) . . ?
C2 N2 Fe 118.1(4) . . ?
O2 N2 Fe 123.3(4) . . ?
C3 N3 O3 118.1(6) . . ?
C3 N3 Fe 118.7(4) . . ?
O3 N3 Fe 122.6(5) . . ?
F B O1 107.6(5) . . ?
F B O3 108.0(5) . . ?
O1 B O3 111.6(5) . . ?
F B O2 108.4(5) . . ?
O1 B O2 111.3(6) . . ?
O3 B O2 109.8(5) . . ?
N1 C1 C2 112.6(5) . 2_655 ?
N1 C1 Cl1 124.4(5) . . ?
C2 C1 Cl1 123.0(4) 2_655 . ?
N2 C2 C1 112.1(5) . 2_655 ?
N2 C2 Cl2 124.1(5) . . ?
C1 C2 Cl2 123.8(4) 2_655 . ?
N3 C3 C3 112.3(4) . 2_655 ?
N3 C3 Cl3 124.4(5) . . ?
C3 C3 Cl3 123.3(3) 2_655 . ?
C7 O4 C4 110.2(16) . . ?
C7 O4A C4 116.4(24) . . ?
C5A C4 O4A 108.0(27) . . ?
C5A C4 O4 117.3(19) . . ?
O4A C4 O4 13.3(34) . . ?
C5A C4 C5 33.2(16) . . ?
O4A C4 C5 85.3(20) . . ?
O4 C4 C5 90.2(14) . . ?
C5A C5 C6 112.0(48) . . ?
C5A C5 C4 48.1(27) . . ?
C6 C5 C4 105.9(21) . . ?
C5A C5 C7 112.2(31) . . ?
C6 C5 C7 46.7(14) . . ?
C4 C5 C7 74.7(12) . . ?
C5 C6 C7 97.0(23) . . ?
C5 C6 C5A 30.6(25) . . ?
C7 C6 C5A 101.3(15) . . ?
O4A C7 O4 13.7(37) . . ?
O4A C7 C6 101.9(27) . . ?
O4 C7 C6 110.1(15) . . ?
O4A C7 C5 82.2(23) . . ?
O4 C7 C5 84.1(15) . . ?
C6 C7 C5 36.3(13) . . ?
C5 C5A C4 98.7(36) . . ?
C5 C5A C6 37.5(26) . . ?
C4 C5A C6 98.1(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe N1 1.901(5) 2_655 ?
Fe N1 1.901(5) . ?
Fe N3 1.914(6) . ?
Fe N3 1.914(6) 2_655 ?
Fe N2 1.915(5) 2_655 ?
Fe N2 1.915(5) . ?
Cl1 C1 1.692(5) . ?
Cl2 C2 1.691(6) . ?
Cl3 C3 1.698(8) . ?
F B 1.349(7) . ?
O1 N1 1.369(6) . ?
O1 B 1.464(8) . ?
O2 N2 1.364(6) . ?
O2 B 1.464(9) . ?
O3 N3 1.376(7) . ?
O3 B 1.465(10) . ?
N1 C1 1.277(8) . ?
N2 C2 1.283(7) . ?
N3 C3 1.267(9) . ?
C1 C2 1.427(8) 2_655 ?
C2 C1 1.427(8) 2_655 ?
C3 C3 1.433(13) 2_655 ?
O4 C7 1.37(2) . ?
O4 C4 1.44(2) . ?
O4A C7 1.26(4) . ?
O4A C4 1.45(4) . ?
C4 C5A 1.35(4) . ?
C4 C5 1.80(4) . ?
C5 C5A 1.00(4) . ?
C5 C6 1.19(3) . ?
C5 C7 2.00(3) . ?
C6 C7 1.47(2) . ?
C6 C5A 1.82(4) . ?
