[MIII2MII3]n+ trigonal bipyramidal cages based on diamagnetic and paramagnetic metalloligands.
Brechin, Euan K.; Sanz, Sergio; O'Connor, Helen; Martí-Centelles, Vicente; Comar, Priyanka; Pitak, Mateusz; Coles, Simon; Lorusso, Giulia; Palacios, Elias; Evangelisti, Marco; Baldansuren, Amgalanbaatar; Chilton, Nicholas F.; Weihe, Høgni; McInnes, Eric J. L.; Lusby, Paul; Piligkos, Stergios; Chem. Sci.  (2017) –; doi:10.1039/C7SC00487G

data_1546080
_publ_section_title
;
 [MIII2MII3]n+ trigonal bipyramidal cages based on diamagnetic and
 paramagnetic metalloligands.
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC00487G
_journal_year                    2017
_chemical_formula_moiety         'C54 H48 Br6 Fe2 N6 O12 Zn3, 2(C N O2)'
_chemical_formula_sum            'C56 H48 Br6 Fe2 N8 O16 Zn3'
_chemical_formula_weight         1876.29
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-05-01 deposited with the CCDC.
2017-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.8153(16)
_cell_length_b                   12.8153(16)
_cell_length_c                   38.817(5)
_cell_measurement_reflns_used    11316
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     5520.9(12)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
SUPERFLIP (Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            32005
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         3.149
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.668
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.816
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Flack x determined using 2506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6717
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0744P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6197
_reflns_number_total             6717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00487g2.cif
_cod_data_source_block           compound2_rev1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5520.9(16)
_cod_database_code               1546080
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4A-C28A
 1.48 with sigma of 0.01
 N4A-O8A
 1.22 with sigma of 0.01
 N4A-O7A
 1.22 with sigma of 0.01
 N4B-C28B
 1.48 with sigma of 0.01
 N4B-O8A
 1.22 with sigma of 0.01
 N4B-O7B
 1.22 with sigma of 0.01
 C28A-C28B
 2.9 with sigma of 0.02
 O7A-C28A
 2.3 with sigma of 0.02
 O8A-C28A
 2.3 with sigma of 0.02
 O8A-O7A
 2.16 with sigma of 0.02
 O7B-C28B
 2.3 with sigma of 0.02
 O8B-C28B
 2.3 with sigma of 0.02
 O8B-O7B
 2.16 with sigma of 0.02
3. Restrained planarity
 N4A, C28A, O7A, O8A
 with sigma of 0.01
 C28B, O7B, N4B, O8B
 with sigma of 0.00001
4. Uiso/Uaniso restraints and constraints
Uiso(O8A) = Uiso(O7A) = Uiso(N4A) = Uiso(C28A)
Uiso(O7B) = Uiso(N4B) = Uiso(O8B) = Uiso(C28B)
5. Others
 Sof(N4B)=Sof(C28B)=Sof(O7B)=Sof(O8B)=1-FVAR(1)
 Sof(N4A)=Sof(C28A)=Sof(O7A)=Sof(O8A)=FVAR(1)
6.a Me refined with riding coordinates:
 C27(H27A,H27B,H27C)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C25(H25), C20(H20), C22(H22), C19(H19), C23(H23)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              12890
_olex2_submission_special_instructions 'No special instructions were received'