#------------------------------------------------------------------------------
#$Date: 2021-10-24 20:53:08 +0300 (Sun, 24 Oct 2021) $
#$Revision: 270074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/25/4332572.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332572
loop_
_publ_author_name
'Cucos, Paula'
'Pascu, Mirela'
'Sessoli, Roberta'
'Avarvari, Narcis'
'Pointillart, Fabrice'
'Andruh, Marius'
_publ_section_title
;
 Heterotopic Helicand for Designing Heterometallic Helicates
;
_journal_issue                   18
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7035
_journal_page_last               7037
_journal_paper_doi               10.1021/ic060533u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         C52H34Co2Fe2N6Na2O26
_chemical_formula_sum            'C52 H34 Co2 Fe2 N6 Na2 O26'
_chemical_formula_weight         1434.39
_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                 123.16
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.896
_cell_length_b                   17.306
_cell_length_c                   17.538
_cell_measurement_reflns_used    45
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     5563.434
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_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  0.1155
_diffrn_reflns_av_sigmaI/netI    0.1274
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26437
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.790245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1659
_refine_ls_R_factor_gt           0.0743
_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)+(0.0000P)²+67.5550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                2949
_reflns_number_total             5431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060533usup1.cif
_cod_data_source_block           p2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C104 H68 Co4 Fe4 N12 Na4 O52'
_cod_original_formula_weight         2868.78
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5563.6
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4332572
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
Co1 Co 0.03399(5) 0.76258(5) 0.17632(6) 0.0203(2) Uani 1 1 d .
Fe1 Fe 0.08673(5) 0.76936(6) 0.05497(6) 0.0220(3) Uani 1 1 d .
O3 O 0.0997(3) 0.6958(3) 0.1544(3) 0.0318(12) Uani 1 1 d .
O1 O 0.1822(2) 0.7254(3) 0.0886(3) 0.0333(12) Uani 1 1 d .
N1 N 0.0252(3) 0.6623(3) 0.2365(4) 0.0218(13) Uani 1 1 d .
O2 O 0.2626(3) 0.6365(4) 0.1131(4) 0.0571(18) Uani 1 1 d .
C3 C 0.2296(4) 0.5432(5) 0.2119(5) 0.037(2) Uani 1 1 d .
H3 H 0.2662 0.5292 0.2029 0.044 Uiso 1 1 calc R
C1 C 0.2131(4) 0.6597(5) 0.1214(5) 0.0300(18) Uani 1 1 d .
C6 C 0.1225(4) 0.5839(4) 0.2425(5) 0.0273(17) Uani 1 1 d .
C2 C 0.1923(4) 0.6114(4) 0.1740(5) 0.0255(17) Uani 1 1 d .
C7 C 0.1375(4) 0.6325(4) 0.1889(4) 0.0220(16) Uani 1 1 d .
C4 C 0.2149(4) 0.4949(5) 0.2627(6) 0.047(2) Uani 1 1 d .
H4 H 0.2404 0.4489 0.2863 0.057 Uiso 1 1 calc R
C8 C 0.0668(4) 0.6016(4) 0.2602(5) 0.0283(18) Uani 1 1 d .
H8 H 0.0598 0.5645 0.2930 0.034 Uiso 1 1 calc R
C5 C 0.1614(4) 0.5165(4) 0.2777(5) 0.035(2) Uani 1 1 d .
H5 H 0.1515 0.4847 0.3124 0.042 Uiso 1 1 calc R
O13 O 0.1016(2) 0.8400(3) 0.1561(3) 0.0229(11) Uani 1 1 d .
N11 N 0.0772(3) 0.8334(3) 0.2923(4) 0.0241(14) Uani 1 1 d .
O11 O 0.0974(3) 0.8612(3) -0.0007(3) 0.0327(12) Uani 1 1 d .
O12 O 0.1167(3) 0.9807(3) -0.0265(4) 0.0507(16) Uani 1 1 d .
C16 C 0.0874(4) 0.9509(4) 0.2243(4) 0.0235(16) Uani 1 1 d .
C12 C 0.0939(4) 0.9639(4) 0.0895(5) 0.0253(16) Uani 1 1 d .
C13 C 0.0863(4) 1.0442(5) 0.0955(6) 0.041(2) Uani 1 1 d .
H13 H 0.0861 1.0760 0.0526 0.049 Uiso 1 1 calc R
C15 C 0.0800(4) 1.0299(4) 0.2249(5) 0.0329(19) Uani 1 1 d .
H15 H 0.0752 1.0520 0.2697 0.039 Uiso 1 1 calc R
C18 C 0.0867(4) 0.9068(4) 0.2937(4) 0.0238(16) Uani 1 1 d .
H18 H 0.0937 0.9338 0.3437 0.029 Uiso 1 1 calc R
C14 C 0.0793(4) 1.0778(5) 0.1608(6) 0.040(2) Uani 1 1 d .
H14 H 0.0743 1.1311 0.1623 0.048 Uiso 1 1 calc R
C11 C 0.1033(4) 0.9349(5) 0.0160(5) 0.0322(19) Uani 1 1 d .
C17 C 0.0940(3) 0.9168(4) 0.1546(4) 0.0217(15) Uani 1 1 d .
O23 O -0.0132(2) 0.7718(3) 0.0370(3) 0.0305(12) Uani 1 1 d .
N21 N -0.0717(3) 0.8034(3) 0.1351(4) 0.0252(14) Uani 1 1 d .
O21 O 0.0355(3) 0.7106(3) -0.0606(3) 0.0334(13) Uani 1 1 d .
C22 C -0.0919(3) 0.7211(4) -0.1135(4) 0.0203(15) Uani 1 1 d .
O22 O -0.0463(3) 0.6665(3) -0.1967(3) 0.0396(14) Uani 1 1 d .
C23 C -0.1632(4) 0.7075(4) -0.1852(5) 0.036(2) Uani 1 1 d .
H23 H -0.1717 0.6852 -0.2384 0.044 Uiso 1 1 calc R
C26 C -0.1402(3) 0.7719(4) -0.0263(4) 0.0238(15) Uani 1 1 d .
C24 C -0.2221(4) 0.7262(5) -0.1794(5) 0.041(2) Uani 1 1 d .
H24 H -0.2694 0.7169 -0.2286 0.049 Uiso 1 1 calc R
C25 C -0.2106(3) 0.7583(5) -0.1018(4) 0.0332(19) Uani 1 1 d .
H25 H -0.2505 0.7714 -0.0989 0.040 Uiso 1 1 calc R
C27 C -0.0797(3) 0.7544(4) -0.0327(4) 0.0238(16) Uani 1 1 d .
C28 C -0.1312(4) 0.8026(4) 0.0561(4) 0.0250(16) Uani 1 1 d .
H28 H -0.1722 0.8237 0.0513 0.030 Uiso 1 1 calc R
C21 C -0.0318(4) 0.6981(4) -0.1258(5) 0.0324(19) Uani 1 1 d .
O31 O 0.1060(4) 0.4569(4) 0.4149(4) 0.0675(19) Uani 1 1 d .
C31 C 0.0658(6) 0.4811(6) 0.4506(7) 0.062(3) Uani 1 1 d .
H31A H 0.0745 0.4456 0.4984 0.075 Uiso 1 1 calc R
H31B H 0.0143 0.4785 0.4029 0.075 Uiso 1 1 calc R
C32 C 0.0831(7) 0.5613(7) 0.4888(7) 0.089(4) Uani 1 1 d .
H32A H 0.0536 0.5738 0.5120 0.134 Uiso 1 1 calc R
H32B H 0.0732 0.5972 0.4416 0.134 Uiso 1 1 calc R
H32C H 0.1337 0.5643 0.5371 0.134 Uiso 1 1 calc R
Na1 Na 0.08893(17) 0.32634(19) 0.3512(2) 0.0448(8) Uani 1 1 d .
O51 O 0.0893(5) 0.1886(4) 0.3404(5) 0.104(3) Uani 1 1 d .
O61 O 0.2180(3) 0.3314(4) 0.4198(4) 0.071(2) Uani 1 1 d .
O71 O 0.2443(4) -0.0071(5) 0.4736(5) 0.105(3) Uani 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'
Co Co 0.3494 0.9721 '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'
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'
Na Na 0.0362 0.0249 '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
O3 Co1 O23 76.66(19) . .
O3 Co1 N1 83.96(19) . .
O23 Co1 N1 122.3(2) . .
O3 Co1 N11 121.4(2) . .
O23 Co1 N11 139.9(2) . .
N1 Co1 N11 96.4(2) . .
O3 Co1 N21 150.5(2) . .
O23 Co1 N21 80.02(18) . .
N1 Co1 N21 93.6(2) . .
N11 Co1 N21 88.0(2) . .
O3 Co1 O13 72.76(17) . .
O23 Co1 O13 72.77(17) . .
N1 Co1 O13 148.80(19) . .
N11 Co1 O13 79.17(18) . .
N21 Co1 O13 116.9(2) . .
O3 Co1 Fe1 44.42(13) . .
O23 Co1 Fe1 43.98(11) . .
N1 Co1 Fe1 125.57(14) . .
N11 Co1 Fe1 122.14(14) . .
N21 Co1 Fe1 121.81(15) . .
O13 Co1 Fe1 43.85(12) . .
O11 Fe1 O21 93.6(2) . .
O11 Fe1 O1 93.8(2) . .
O21 Fe1 O1 91.3(2) . .
O11 Fe1 O13 86.55(19) . .
O21 Fe1 O13 159.31(19) . .
O1 Fe1 O13 109.35(19) . .
O11 Fe1 O23 108.7(2) . .
O21 Fe1 O23 83.81(18) . .
O1 Fe1 O23 157.3(2) . .
O13 Fe1 O23 76.59(18) . .
O11 Fe1 O3 159.4(2) . .
O21 Fe1 O3 106.8(2) . .
O1 Fe1 O3 82.85(19) . .
O13 Fe1 O3 75.54(18) . .
O23 Fe1 O3 77.4(2) . .
O11 Fe1 Co1 126.96(14) . .
O21 Fe1 Co1 119.73(14) . .
O1 Fe1 Co1 122.58(14) . .
O13 Fe1 Co1 47.72(12) . .
O23 Fe1 Co1 45.13(12) . .
O3 Fe1 Co1 44.20(13) . .
C7 O3 Co1 136.2(4) . .
C7 O3 Fe1 132.4(4) . .
Co1 O3 Fe1 91.38(19) . .
C1 O1 Fe1 132.9(4) . .
C8 N1 N1 115.6(4) . 2
C8 N1 Co1 126.0(4) . .
N1 N1 Co1 118.1(2) 2 .
C2 C3 C4 122.9(7) . .
O2 C1 O1 121.0(7) . .
O2 C1 C2 118.3(7) . .
O1 C1 C2 120.6(6) . .
C5 C6 C7 119.1(6) . .
C5 C6 C8 118.1(6) . .
C7 C6 C8 122.8(6) . .
C3 C2 C7 118.1(6) . .
C3 C2 C1 118.6(6) . .
C7 C2 C1 123.3(6) . .
O3 C7 C2 121.3(6) . .
O3 C7 C6 118.9(6) . .
C2 C7 C6 119.8(6) . .
C3 C4 C5 118.6(7) . .
N1 C8 C6 129.0(6) . .
C6 C5 C4 121.6(7) . .
C17 O13 Fe1 128.6(4) . .
C17 O13 Co1 121.9(4) . .
Fe1 O13 Co1 88.43(17) . .
C18 N11 N21 115.5(5) . 2
C18 N11 Co1 125.2(4) . .
N21 N11 Co1 115.7(4) 2 .
C11 O11 Fe1 135.6(4) . .
C15 C16 C17 118.9(6) . .
C15 C16 C18 117.6(6) . .
C17 C16 C18 123.5(6) . .
C17 C12 C13 117.4(6) . .
C17 C12 C11 124.4(7) . .
C13 C12 C11 118.1(6) . .
C14 C13 C12 123.6(7) . .
C16 C15 C14 122.3(7) . .
N11 C18 C16 125.7(6) . .
C13 C14 C15 117.9(7) . .
O12 C11 O11 121.8(7) . .
O12 C11 C12 119.7(7) . .
O11 C11 C12 118.6(6) . .
O13 C17 C12 122.5(6) . .
O13 C17 C16 117.6(6) . .
C12 C17 C16 119.8(6) . .
C27 O23 Fe1 133.2(4) . .
C27 O23 Co1 131.0(4) . .
Fe1 O23 Co1 90.89(17) . .
C28 N21 N11 115.7(5) . 2
C28 N21 Co1 129.5(5) . .
N11 N21 Co1 114.8(4) 2 .
C21 O21 Fe1 136.4(4) . .
C21 O21 Na1 95.8(4) . 6_565
Fe1 O21 Na1 125.1(2) . 6_565
C23 C22 C27 118.7(6) . .
C23 C22 C21 117.7(6) . .
C27 C22 C21 123.6(6) . .
C21 O22 Na1 150.1(5) . 5_565
C21 O22 Na1 91.9(5) . 6_565
Na1 O22 Na1 91.91(19) 5_565 6_565
C24 C23 C22 121.6(7) . .
C25 C26 C27 118.8(6) . .
C25 C26 C28 119.1(6) . .
C27 C26 C28 122.1(6) . .
C25 C24 C23 119.9(7) . .
C24 C25 C26 121.5(6) . .
O23 C27 C22 121.8(6) . .
O23 C27 C26 118.7(5) . .
C22 C27 C26 119.5(6) . .
N21 C28 C26 125.9(6) . .
O22 C21 O21 120.5(7) . .
O22 C21 C22 120.1(7) . .
O21 C21 C22 119.4(6) . .
O22 C21 Na1 63.2(4) . 6_565
O21 C21 Na1 57.9(3) . 6_565
C22 C21 Na1 172.9(5) . 6_565
C31 O31 Na1 120.3(6) . .
O31 C31 C32 114.3(9) . .
O22 Na1 O51 88.7(2) 5_565 .
O22 Na1 O61 101.2(2) 5_565 .
O51 Na1 O61 91.2(3) . .
O22 Na1 O31 110.1(2) 5_565 .
O51 Na1 O31 161.1(3) . .
O61 Na1 O31 83.9(2) . .
O22 Na1 O21 135.4(2) 5_565 6_566
O51 Na1 O21 79.4(2) . 6_566
O61 Na1 O21 121.8(2) . 6_566
O31 Na1 O21 87.7(2) . 6_566
O22 Na1 O22 87.80(19) 5_565 6_566
O51 Na1 O22 94.3(3) . 6_566
O61 Na1 O22 169.6(2) . 6_566
O31 Na1 O22 88.1(2) . 6_566
O21 Na1 O22 51.05(16) 6_566 6_566
O22 Na1 C21 110.5(2) 5_565 6_566
O51 Na1 C21 84.8(3) . 6_566
O61 Na1 C21 147.9(3) . 6_566
O31 Na1 C21 89.7(2) . 6_566
O21 Na1 C21 26.28(18) 6_566 6_566
O22 Na1 C21 24.92(18) 6_566 6_566
O22 Na1 Na1 47.01(14) 5_565 2
O51 Na1 Na1 88.3(2) . 2
O61 Na1 Na1 148.2(2) . 2
O31 Na1 Na1 105.39(18) . 2
O21 Na1 Na1 89.41(17) 6_566 2
O22 Na1 Na1 41.07(12) 6_566 2
C21 Na1 Na1 63.70(18) 6_566 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.041(5) .
Co1 O23 2.074(4) .
Co1 N1 2.095(6) .
Co1 N11 2.105(6) .
Co1 N21 2.133(6) .
Co1 O13 2.166(4) .
Co1 Fe1 2.9265(11) .
Fe1 O11 1.945(5) .
Fe1 O21 1.978(5) .
Fe1 O1 1.987(5) .
Fe1 O13 2.028(4) .
Fe1 O23 2.032(4) .
Fe1 O3 2.049(5) .
O3 C7 1.305(8) .
O1 C1 1.287(8) .
N1 C8 1.301(8) .
N1 N1 1.417(10) 2
O2 C1 1.238(8) .
C3 C2 1.380(10) .
C3 C4 1.382(10) .
C1 C2 1.489(9) .
C6 C5 1.376(10) .
C6 C7 1.426(9) .
C6 C8 1.446(9) .
C2 C7 1.409(9) .
C4 C5 1.385(10) .
O13 C17 1.337(8) .
N11 C18 1.285(8) .
N11 N21 1.439(7) 2
O11 C11 1.300(9) .
O12 C11 1.227(8) .
C16 C15 1.378(10) .
C16 C17 1.433(9) .
C16 C18 1.445(9) .
C12 C17 1.403(9) .
C12 C13 1.409(10) .
C12 C11 1.500(10) .
C13 C14 1.367(11) .
C15 C14 1.390(10) .
O23 C27 1.325(7) .
N21 C28 1.281(8) .
N21 N11 1.439(7) 2
O21 C21 1.297(9) .
O21 Na1 2.481(5) 6_565
C22 C23 1.389(9) .
C22 C27 1.414(8) .
C22 C21 1.499(9) .
O22 C21 1.229(8) .
O22 Na1 2.337(6) 5_565
O22 Na1 2.602(6) 6_565
C23 C24 1.387(10) .
C26 C25 1.398(9) .
C26 C27 1.423(8) .
C26 C28 1.449(9) .
C24 C25 1.360(10) .
C21 Na1 2.915(8) 6_565
O31 C31 1.396(10) .
O31 Na1 2.457(7) .
C31 C32 1.496(13) .
Na1 O22 2.337(6) 5_565
Na1 O51 2.392(8) .
Na1 O61 2.393(7) .
Na1 O21 2.481(5) 6_566
Na1 O22 2.602(6) 6_566
Na1 C21 2.915(8) 6_566
Na1 Na1 3.556(6) 2
