Discrete polynuclear manganese(ii) complexes with thiacalixarene ligands: synthesis, structures and photophysical properties.
Suffren, Yan; O'Toole, Niall; Hauser, Andreas; Jeanneau, Erwann; Brioude, Arnaud; Desroches, Cédric; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7991–8000; doi:10.1039/c5dt00827a

data_7034550
_publ_section_title
;
 Discrete polynuclear manganese(ii) complexes with thiacalixarene ligands:
 synthesis, structures and photophysical properties.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7991
_journal_page_last               8000
_journal_paper_doi               10.1039/c5dt00827a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C80 H88 F Mn4 O24 S8, C14 H30 K O8, 2(C H4 O)'
_chemical_formula_sum            'C96 H126 F K Mn4 O34 S8'
_chemical_formula_weight         2358.31
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   difmap
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_audit_update_record
;
2015-02-19 deposited with the CCDC.
2015-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                101.431(4)
_cell_angle_beta                 99.543(6)
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_cell_length_a                   12.0143(9)
_cell_length_b                   12.3064(7)
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_cell_measurement_reflns_used    19966
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.3650
_cell_measurement_theta_min      3.5310
_cell_volume                     2607.8(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_limit_l_min       -25
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_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.756
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1230.000
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.24
_refine_diff_density_min         -0.95
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13282
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.0008117
_refine_ls_shift/su_mean         0.0000284
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 463. 674. 348. 88.5 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1250
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1250
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10415
_reflns_number_total             13313
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0711
_oxford_refine_ls_scale          1.906(7)
_oxford_reflns_number_all        13282
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c5dt00827a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7034550.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7034550