#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:09:15 +0100 (vie 25 de mar de 2016) $
#$Revision: 179954 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/49/7024998.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_7024998
loop_
_publ_author_name
'Mason, Kevin'
'Gass, Ian A.'
'Parsons, Simon'
'Collins, Anna'
'White, Fraser J.'
'Slawin, Alexandra M. Z.'
'Brechin, Euan K.'
'Tasker, Peter A.'
_publ_section_title
;
 Building Fe(III) clusters with derivatised salicylaldoximes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2727
_journal_page_last               2734
_journal_paper_doi               10.1039/b924143d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C57 H84 Fe6 N6 Na3 O29. MeOH'
_chemical_formula_sum            'C58 H88 Fe6 N6 Na3 O30'
_chemical_formula_weight         1753.41
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-10-13
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.40610(10)
_cell_length_b                   12.40610(10)
_cell_length_c                   28.8478(6)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    150
_cell_measurement_theta_max      56
_cell_measurement_theta_min      5
_cell_volume                     3845.16(9)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            46897
_diffrn_reflns_theta_full        27.857
_diffrn_reflns_theta_max         29.018
_diffrn_reflns_theta_min         1.412
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.51
_exptl_crystal_description       block
_exptl_crystal_F_000             1814.000
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
A disordered MeOH group was squeezed, as the disorder could not be
modelled satisfactorilly.
;
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.41
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9647
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2110
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002562
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
1.54 0.577 1.27
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0375
_refine_ls_wR_factor_gt          0.0322
_refine_ls_wR_factor_ref         0.0322
_reflns_limit_h_max              0
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              39
_reflns_limit_l_min              0
_reflns_number_gt                2110
_reflns_number_total             3379
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2484(5)
_oxford_structure_analysis_title 'eb6113 in P6(3)/m'
_cod_data_source_file            b924143d.txt
_cod_data_source_block           eb6113
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 63/m '
_cod_database_code               7024998
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x-y,x,z+1/2
-x+y,-x,-z+1/2
-y,x-y,z
y,-x+y,-z
-x,-y,z+1/2
x,y,-z+1/2
-x+y,-x,z
x-y,x,-z
y,-x+y,z+1/2
-y,x-y,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.70995(2) 0.51065(2) 0.695670(8) 0.0121 1.0000 Uani . .
Na1 Na 1.00336(11) 0.79034(11) 0.7500 0.0234 1.0000 Uani S T
C3 C 0.56411(19) 0.4818(2) 0.60585(7) 0.0195 1.0000 Uani . .
C4 C 0.4692(3) 0.4036(2) 0.57004(8) 0.0371 1.0000 Uani . .
C5 C 0.6543(2) 0.6133(2) 0.59584(7) 0.0200 1.0000 Uani . .
C6 C 0.73272(18) 0.69978(19) 0.62982(7) 0.0178 1.0000 Uani . .
C7 C 0.8071(2) 0.82589(19) 0.61705(8) 0.0227 1.0000 Uani . .
C8 C 0.8047(2) 0.8659(2) 0.57242(9) 0.0289 1.0000 Uani . .
C9 C 0.7312(2) 0.7817(2) 0.53885(9) 0.0319 1.0000 Uani . .
C10 C 0.5253(3) 0.5616(3) 0.7500 0.0205 1.0000 Uani S T
C20 C 1.1617(2) 0.7249(2) 0.66126(11) 0.0377 1.0000 Uani . .
C21 C 0.6575(2) 0.6578(2) 0.55076(8) 0.0293 1.0000 Uani . .
N2 N 0.56586(15) 0.43397(15) 0.64563(6) 0.0155 1.0000 Uani . .
O1 O 0.47122(13) 0.31371(13) 0.65271(5) 0.0164 1.0000 Uani . .
O2 O 0.82824(17) 0.57617(18) 0.7500 0.0132 1.0000 Uani DS T
O3 O 0.6667 0.3333 0.70715(8) 0.0122 1.0000 Uani S T
O4 O 1.16955(19) 0.9979(2) 0.7500 0.0215 1.0000 Uani DS T
O6 O 0.73675(13) 0.66961(13) 0.67379(5) 0.0179 1.0000 Uani . .
O10 O 0.59590(17) 0.49985(18) 0.7500 0.0140 1.0000 Uani S T
O20 O 1.06124(16) 0.72620(16) 0.68370(6) 0.0323 1.0000 Uani D .
H2 H 0.870(3) 0.542(3) 0.7500 0.0196 1.0000 Uiso DS .
H4 H 1.212(2) 1.011(3) 0.7730(7) 0.0293 1.0000 Uiso D .
H20 H 0.9965(19) 0.674(3) 0.6714(12) 0.0423 1.0000 Uiso D .
H201 H 1.1621 0.7393 0.6283 0.0556 1.0000 Uiso . .
H202 H 1.1564 0.6459 0.6637 0.0544 1.0000 Uiso . .
H203 H 1.2404 0.7904 0.6729 0.0552 1.0000 Uiso . .
H41 H 0.4173 0.3215 0.5810 0.0495 1.0000 Uiso . .
H42 H 0.4197 0.4415 0.5628 0.0493 1.0000 Uiso . .
H43 H 0.5106 0.3997 0.5430 0.0490 1.0000 Uiso . .
H71 H 0.8561 0.8816 0.6387 0.0271 1.0000 Uiso . .
H81 H 0.8527 0.9493 0.5655 0.0339 1.0000 Uiso . .
H91 H 0.7328 0.8091 0.5087 0.0380 1.0000 Uiso . .
H211 H 0.6062 0.6029 0.5289 0.0339 1.0000 Uiso . .
H102 H 0.5779 0.6497 0.7500 0.0363 1.0000 Uiso . .
H103 H 0.4738 0.5388 0.7764 0.0359 1.0000 Uiso . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 9_665 Fe1 N2 . 95.22(6) yes
O1 9_665 Fe1 O2 . 92.58(6) yes
N2 . Fe1 O2 . 172.01(6) yes
O1 9_665 Fe1 O3 . 88.83(6) yes
N2 . Fe1 O3 . 85.25(6) yes
O2 . Fe1 O3 . 93.17(7) yes
O1 9_665 Fe1 O6 . 88.30(6) yes
N2 . Fe1 O6 . 84.94(6) yes
O2 . Fe1 O6 . 97.07(7) yes
O3 . Fe1 O6 . 169.48(7) yes
O1 9_665 Fe1 O10 . 169.41(6) yes
N2 . Fe1 O10 . 95.22(6) yes
O2 . Fe1 O10 . 76.94(6) yes
O3 . Fe1 O10 . 90.26(7) yes
O6 . Fe1 O10 . 94.39(7) yes
O20 8_556 Na1 O4 4_676 121.72(6) yes
O20 8_556 Na1 O2 . 83.50(6) yes
O4 4_676 Na1 O2 . 79.95(7) yes
O20 8_556 Na1 O4 . 97.06(6) yes
O4 4_676 Na1 O4 . 99.05(11) yes
O2 . Na1 O4 . 179.00(9) yes
O20 8_556 Na1 O20 . 111.12(11) yes
O4 4_676 Na1 O20 . 121.72(6) yes
O2 . Na1 O20 . 83.50(6) yes
O4 . Na1 O20 . 97.06(6) yes
C4 . C3 C5 . 119.81(18) yes
C4 . C3 N2 . 120.0(2) yes
C5 . C3 N2 . 120.18(18) yes
C3 . C4 H41 . 110.9 no
C3 . C4 H42 . 108.6 no
H41 . C4 H42 . 109.9 no
C3 . C4 H43 . 109.2 no
H41 . C4 H43 . 108.3 no
H42 . C4 H43 . 109.8 no
C3 . C5 C6 . 123.76(18) yes
C3 . C5 C21 . 118.20(19) yes
C6 . C5 C21 . 117.91(19) yes
C5 . C6 C7 . 118.62(19) yes
C5 . C6 O6 . 123.62(18) yes
C7 . C6 O6 . 117.71(19) yes
C6 . C7 C8 . 121.3(2) yes
C6 . C7 H71 . 119.0 no
C8 . C7 H71 . 119.6 no
C7 . C8 C9 . 120.4(2) yes
C7 . C8 H81 . 119.0 no
C9 . C8 H81 . 120.6 no
C8 . C9 C21 . 119.1(2) yes
C8 . C9 H91 . 119.6 no
C21 . C9 H91 . 121.3 no
H103 8_556 C10 O10 . 110.2 no
H103 8_556 C10 H102 . 108.6 no
O10 . C10 H102 . 111.4 no
H103 8_556 C10 H103 . 107.8 no
O10 . C10 H103 . 110.2 no
H102 . C10 H103 . 108.6 no
O20 . C20 H201 . 111.7 no
O20 . C20 H202 . 111.7 no
H201 . C20 H202 . 104.9 no
O20 . C20 H203 . 110.9 no
H201 . C20 H203 . 106.2 no
H202 . C20 H203 . 111.2 no
C5 . C21 C9 . 122.7(2) yes
C5 . C21 H211 . 118.3 no
C9 . C21 H211 . 119.0 no
Fe1 . N2 C3 . 126.94(14) yes
Fe1 . N2 O1 . 117.18(11) yes
C3 . N2 O1 . 115.27(16) yes
N2 . O1 Fe1 5_655 121.93(11) yes
Na1 . O2 Fe1 8_556 120.54(6) yes
Na1 . O2 Fe1 . 120.54(6) yes
Fe1 8_556 O2 Fe1 . 101.82(8) yes
Na1 . O2 H2 . 96(3) no
Fe1 8_556 O2 H2 . 108.3(16) no
Fe1 . O2 H2 . 108.3(16) no
Fe1 . O3 Fe1 5_655 117.35(3) yes
Fe1 . O3 Fe1 9_665 117.35(3) yes
Fe1 5_655 O3 Fe1 9_665 117.35(3) yes
Na1 . O4 Na1 5_765 140.95(11) yes
Na1 . O4 H4 8_556 110(2) no
Na1 5_765 O4 H4 8_556 92(2) no
Na1 . O4 H4 . 110(2) no
Na1 5_765 O4 H4 . 92(2) no
H4 8_556 O4 H4 . 109(4) no
C6 . O6 Fe1 . 125.90(13) yes
C10 . O10 Fe1 . 123.35(8) yes
C10 . O10 Fe1 8_556 123.35(8) yes
Fe1 . O10 Fe1 8_556 98.40(8) yes
Na1 . O20 C20 . 143.96(16) yes
Na1 . O20 H20 . 106(3) no
C20 . O20 H20 . 108(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O1 9_665 1.9800(14) yes
Fe1 N2 . 2.1174(16) yes
Fe1 O2 . 2.0194(12) yes
Fe1 O3 . 2.0140(4) yes
Fe1 O6 . 1.9345(14) yes
Fe1 O10 . 2.0704(12) yes
Na1 O20 8_556 2.3192(19) yes
Na1 O4 4_676 2.458(3) yes
Na1 O2 . 2.451(2) yes
Na1 O4 . 2.361(2) yes
Na1 O20 . 2.3192(19) yes
C3 C4 . 1.501(3) yes
C3 C5 . 1.474(3) yes
C3 N2 . 1.297(3) yes
C4 H41 . 0.947 no
C4 H42 . 0.965 no
C4 H43 . 0.948 no
C5 C6 . 1.419(3) yes
C5 C21 . 1.406(3) yes
C6 C7 . 1.411(3) yes
C6 O6 . 1.330(2) yes
C7 C8 . 1.385(3) yes
C7 H71 . 0.904 no
C8 C9 . 1.381(4) yes
C8 H81 . 0.921 no
C9 C21 . 1.383(4) yes
C9 H91 . 0.930 no
C10 H103 8_556 0.942 no
C10 O10 . 1.423(3) yes
C10 H102 . 0.952 no
C10 H103 . 0.942 no
C20 O20 . 1.412(3) yes
C20 H201 . 0.966 no
C20 H202 . 0.950 no
C20 H203 . 0.966 no
C21 H211 . 0.913 no
N2 O1 . 1.376(2) yes
O2 H2 . 0.818(10) no
O4 H4 8_556 0.815(9) no
O4 H4 . 0.815(9) no
O20 H20 . 0.819(10) no
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 6.6 -0.2
2 0.000 0.000 0.500 6.6 -0.1
3 0.333 0.667 0.534 90.1 16.5
4 0.333 0.667 0.966 90.1 17.3
5 0.333 0.667 0.750 27.0 -0.9
6 0.667 0.333 0.034 90.1 17.2
7 0.667 0.333 0.466 90.0 16.9
8 0.667 0.333 0.250 27.0 -0.9
