#------------------------------------------------------------------------------
#$Date: 2018-11-22 11:36:32 +0200 (Thu, 22 Nov 2018) $
#$Revision: 212110 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/21/62/7216224.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_7216224
loop_
_publ_author_name
'Wang, Lei'
'Wang, Wenqiang'
'Guo, Dong'
'Zhang, Ao'
'Song, Yaoguang'
'Zhang, Yiheng'
'Huang, Keke'
_publ_section_title
;
 Design and syntheses of hybrid supramolecular architectures: based on
 [Fe(C2O4)3]3− metallotectons and diverse organic cations
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              5437
_journal_paper_doi               10.1039/c4ce00357h
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C22 H24 Fe K N4 O14'
_chemical_formula_weight         663.40
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.412(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7637(12)
_cell_length_b                   20.5458(15)
_cell_length_c                   9.5211(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2755.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.836
_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  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5284
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.775
_exptl_crystal_colour            emerald
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+2.8996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                2736
_reflns_number_total             3103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00357h2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

2018-11-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C88 H96 Fe4 K4 N16 O56'
_cod_original_formula_weight         2653.61
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7216224
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.0000 0.172311(16) -0.7500 0.02228(10) Uani 1 2 d S
K1 K 0.0000 0.12581(3) -0.2500 0.03424(15) Uani 1 2 d S
O1 O -0.10406(10) 0.23951(7) -0.79960(14) 0.0373(3) Uani 1 1 d .
O2 O -0.18479(13) 0.30368(9) -0.69047(18) 0.0584(5) Uani 1 1 d .
O3 O -0.10988(10) 0.23290(7) -0.43558(15) 0.0370(3) Uani 1 1 d .
O4 O -0.02407(9) 0.17936(6) -0.55264(13) 0.0288(3) Uani 1 1 d .
O5 O -0.08634(8) 0.09890(6) -0.83873(13) 0.0263(3) Uani 1 1 d .
O6 O -0.08787(10) -0.00865(7) -0.85840(18) 0.0458(4) Uani 1 1 d .
O7 O 0.17330(13) 0.10971(9) -0.33650(19) 0.0499(4) Uani 1 1 d .
C1 C -0.05030(11) 0.04201(8) -0.80744(18) 0.0249(3) Uani 1 1 d .
C2 C -0.13013(13) 0.25931(9) -0.6906(2) 0.0319(4) Uani 1 1 d .
C3 C -0.08554(12) 0.22150(8) -0.54553(19) 0.0251(3) Uani 1 1 d .
N1 N -0.29553(10) 0.15488(8) -0.60636(16) 0.0297(3) Uani 1 1 d .
H1 H -0.3079 0.1876 -0.5588 0.036 Uiso 1 1 d R
N2 N -0.29149(10) 0.09193(7) -0.78345(16) 0.0259(3) Uani 1 1 d .
C4 C -0.38075(19) 0.19694(12) -0.8582(3) 0.0525(6) Uani 1 1 d .
H4A H -0.4460 0.1834 -0.8909 0.079 Uiso 1 1 calc R
H4B H -0.3568 0.2000 -0.9412 0.079 Uiso 1 1 calc R
H4C H -0.3762 0.2387 -0.8112 0.079 Uiso 1 1 calc R
C5 C -0.32419(12) 0.14869(9) -0.7522(2) 0.0286(4) Uani 1 1 d .
C6 C -0.24354(12) 0.10161(9) -0.5432(2) 0.0300(4) Uani 1 1 d .
H6 H -0.2157 0.0943 -0.4432 0.036 Uiso 1 1 calc R
C7 C -0.24062(12) 0.06212(9) -0.6536(2) 0.0294(4) Uani 1 1 d .
H7 H -0.2100 0.0221 -0.6447 0.035 Uiso 1 1 calc R
C8 C -0.31518(13) 0.06204(11) -0.9309(2) 0.0363(4) Uani 1 1 d .
H8A H -0.2670 0.0303 -0.9331 0.044 Uiso 1 1 calc R
H8B H -0.3159 0.0953 -1.0036 0.044 Uiso 1 1 calc R
C9 C -0.41109(13) 0.02919(10) -0.9688(2) 0.0338(4) Uani 1 1 d .
C10 C -0.42136(14) -0.02949(11) -0.9058(2) 0.0416(5) Uani 1 1 d .
H10 H -0.3686 -0.0497 -0.8421 0.050 Uiso 1 1 calc R
C11 C -0.49034(15) 0.05861(11) -1.0633(2) 0.0417(5) Uani 1 1 d .
H11 H -0.4842 0.0983 -1.1065 0.050 Uiso 1 1 calc R
H7A H 0.213(2) 0.1376(14) -0.314(3) 0.062(9) Uiso 1 1 d .
H7B H 0.147(2) 0.1109(14) -0.427(4) 0.067(9) Uiso 1 1 d .
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
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
O5 Fe1 O5 81.58(7) . 2_553
O5 Fe1 O1 164.78(5) . 2_553
O5 Fe1 O1 94.20(5) 2_553 2_553
O5 Fe1 O1 94.20(5) . .
O5 Fe1 O1 164.78(5) 2_553 .
O1 Fe1 O1 93.43(9) 2_553 .
O5 Fe1 O4 85.88(5) . 2_553
O5 Fe1 O4 100.40(5) 2_553 2_553
O1 Fe1 O4 80.49(5) 2_553 2_553
O1 Fe1 O4 93.84(5) . 2_553
O5 Fe1 O4 100.40(5) . .
O5 Fe1 O4 85.88(5) 2_553 .
O1 Fe1 O4 93.84(5) 2_553 .
O1 Fe1 O4 80.49(5) . .
O4 Fe1 O4 171.77(7) 2_553 .
C2 O1 Fe1 114.97(11) . .
C3 O4 Fe1 115.20(11) . .
C1 O5 Fe1 115.05(10) . .
H7A O7 H7B 109(3) . .
O6 C1 O5 125.61(15) . .
O6 C1 C1 120.48(10) . 2_553
O5 C1 C1 113.90(9) . 2_553
O2 C2 O1 126.88(18) . .
O2 C2 C3 118.67(17) . .
O1 C2 C3 114.45(15) . .
O3 C3 O4 124.88(17) . .
O3 C3 C2 120.66(15) . .
O4 C3 C2 114.46(15) . .
C5 N1 C6 110.09(15) . .
C5 N1 H1 124.9 . .
C6 N1 H1 125.0 . .
C5 N2 C7 108.95(15) . .
C5 N2 C8 125.44(16) . .
C7 N2 C8 125.24(16) . .
C5 C4 H4A 109.5 . .
C5 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C5 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N2 C5 N1 107.11(15) . .
N2 C5 C4 127.05(18) . .
N1 C5 C4 125.84(18) . .
C7 C6 N1 106.58(16) . .
C7 C6 H6 126.7 . .
N1 C6 H6 126.7 . .
C6 C7 N2 107.28(16) . .
C6 C7 H7 126.4 . .
N2 C7 H7 126.4 . .
N2 C8 C9 110.57(15) . .
N2 C8 H8A 109.5 . .
C9 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
C9 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
C10 C9 C11 118.99(19) . .
C10 C9 C8 120.35(19) . .
C11 C9 C8 120.6(2) . .
C9 C10 C11 120.4(2) . 5_453
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 5_453 .
C9 C11 C10 120.6(2) . 5_453
C9 C11 H11 119.7 . .
C10 C11 H11 119.7 5_453 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O5 1.9922(12) .
Fe1 O5 1.9922(12) 2_553
Fe1 O1 2.0138(13) 2_553
Fe1 O1 2.0138(13) .
Fe1 O4 2.0194(12) 2_553
Fe1 O4 2.0194(12) .
O1 C2 1.277(2) .
O2 C2 1.218(2) .
O3 C3 1.227(2) .
O4 C3 1.271(2) .
O5 C1 1.282(2) .
O6 C1 1.211(2) .
O7 H7A 0.81(3) .
O7 H7B 0.83(3) .
C1 C1 1.559(3) 2_553
C2 C3 1.549(2) .
N1 C5 1.331(2) .
N1 C6 1.368(2) .
N1 H1 0.8605 .
N2 C5 1.330(2) .
N2 C7 1.383(2) .
N2 C8 1.475(2) .
C4 C5 1.481(3) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C6 C7 1.339(3) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 C9 1.512(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.375(3) .
C9 C11 1.384(3) .
C10 C11 1.384(3) 5_453
C10 H10 0.9300 .
C11 C10 1.384(3) 5_453
C11 H11 0.9300 .
