Tetranuclear manganese(ii) complexes of sulfonylcalix[4]arene macrocycles: synthesis, structure, spectroscopic and magnetic properties.
Lamouchi, Meriem; Jeanneau, Erwann; Pillonnet, Anne; Brioude, Arnaud; Martini, Matteo; Stéphan, Olivier; Meganem, Faouzi; Novitchi, Ghenadie; Luneau, Dominique; Desroches, Cédric; Dalton transactions (Cambridge, England : 2003) 41 (2012) 2707–2713; doi:10.1039/c2dt11786j

data_7018183
_publ_section_title
;
 Tetranuclear manganese(ii) complexes of sulfonylcalix[4]arene
 macrocycles: synthesis, structure, spectroscopic and magnetic properties.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2707
_journal_page_last               2713
_journal_paper_doi               10.1039/c2dt11786j
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C82 H96 F K Mn4 O26 S8, 3.3(C H4 O'
_chemical_formula_sum            'C85.3 H109.18 F K Mn4 O29.3 S8'
_chemical_formula_weight         2137.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                72.172(5)
_cell_angle_beta                 81.666(4)
_cell_angle_gamma                64.773(5)
_cell_formula_units_Z            1
_cell_length_a                   12.1491(6)
_cell_length_b                   12.9634(7)
_cell_length_c                   17.3393(9)
_cell_measurement_reflns_used    20983
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.5545
_cell_measurement_theta_min      3.3178
_cell_volume                     2351.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59479
_diffrn_reflns_theta_full        26.665
_diffrn_reflns_theta_max         29.617
_diffrn_reflns_theta_min         3.324
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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            colorless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1111.328
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.074
_refine_diff_density_max         2.48
_refine_diff_density_min         -1.38
_refine_ls_extinction_coef       124(9)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         11882
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.0006035
_refine_ls_shift/su_mean         0.0000319
_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:
680. 0.104E+04 547. 145.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1617
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1617
_reflns_limit_h_max              16
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                9549
_reflns_number_total             11882
_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   0.0795
_oxford_refine_ls_scale          2.108(16)
_oxford_reflns_number_all        11882
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c2dt11786j.txt
_cod_data_source_block           KF
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C85.30 H109.18 F K Mn4 O29.30 S8'
_cod_database_code               7018183
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) H ( 213,X'S)
RIDE C ( 22,X'S) H ( 222,X'S) H ( 221,X'S) H ( 223,X'S)
RIDE C ( 23,X'S) H ( 231,X'S) H ( 233,X'S) H ( 232,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 39,X'S) H ( 391,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S)
RIDE C ( 46,X'S) H ( 461,X'S)
RIDE C ( 48,X'S) H ( 481,X'S)
RIDE C ( 50,X'S) H ( 501,X'S) H ( 503,X'S) H ( 502,X'S)
RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) H ( 513,X'S)
RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) H ( 523,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 55,X'S) H ( 551,X'S)
RIDE C ( 57,X'S) H ( 571,X'S) H ( 573,X'S) H ( 572,X'S)
RIDE C ( 58,X'S) H ( 581,X'S) H ( 583,X'S) H ( 582,X'S)
RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) H ( 593,X'S)
RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) H ( 613,X'S)
RIDE O ( 62,X'S) H ( 621,X'S)
RIDE C ( 63,X'S) H ( 631,X'S) H ( 633,X'S) H ( 632,X'S)
RIDE O ( 64,X'S) H ( 641,X'S)
RIDE C ( 65,X'S) H ( 651,X'S) H ( 652,X'S) H ( 653,X'S)
RIDE O ( 66,X'S) H ( 661,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
U(IJ)'S 0.0, 0.010000 = C(61) TO O(62)
DISTANCE 1.550000 , 0.010000 = C(61) TO O(62)
DISTANCE 1.550000 , 0.010000 = C(65) TO O(66)
DISTANCE 1.550000 , 0.010000 = C(63) TO O(64)
END
;