Syntheses, structures and photocatalytic properties of five new praseodymium-antimony oxochlorides: from discrete clusters to 3D inorganic-organic hybrid racemic compounds.
Zou, Guo-Dong; Wang, Ze-Ping; Song, Ying; Hu, Bing; Huang, Xiao-Ying; Dalton transactions (Cambridge, England : 2003) 43 (2014) 10064–10073; doi:10.1039/c4dt00771a

data_7030869
_publ_section_title
;
 Syntheses, structures and photocatalytic properties of five new
 praseodymium-antimony oxochlorides: from discrete clusters to 3D
 inorganic-organic hybrid racemic compounds.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10064
_journal_page_last               10073
_journal_paper_doi               10.1039/c4dt00771a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'6(C6 H8 N),10(C36 H24 Fe N6 2+), C60 H30 N24 Cl53 O146 Pr20 Sb60,110(H2 O)'
_chemical_formula_sum            'C456 H538 Cl53 Fe10 N90 O256 Pr20 Sb60'
_chemical_formula_weight         23936.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
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_audit_creation_method           SHELXL-2014
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   59.1220(7)
_cell_length_b                   59.1220(7)
_cell_length_c                   39.2567(3)
_cell_measurement_reflns_used    24970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9440
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_cell_volume                     137218(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Windows Word 2003'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3503
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -71
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            197391
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
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_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    33.345
_exptl_absorpt_correction_T_max  0.112
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             90824
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_platon_squeeze_details
; 
The 110 water guest molecules have been included into the formula on the 
basis of these calculations, as well as the EA and TGA analyses
;
_refine_diff_density_max         3.466
_refine_diff_density_min         -2.201
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4042
_refine_ls_number_reflns         62536
_refine_ls_number_restraints     7852
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.1379
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+9999.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2414
_refine_ls_wR_factor_ref         0.2598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33568
_reflns_number_total             62536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00771a2.cif
_cod_data_source_block           compound-5
_cod_depositor_comments
'Adding full bibliography for 7030865--7030869.cif.'
_cod_database_code               7030869
_shelxl_version_number           2014-3
_shelx_res_checksum              96167