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_7018184
_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 H97 K Mn4 O27 S8, C0.61 H2.46 O0.61, 2.92(C H4 O)
;
_chemical_formula_sum            'C85.53 H111.12 K Mn4 O30.53 S8'
_chemical_formula_weight         2143.13
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.222(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2087(4)
_cell_length_b                   18.8106(5)
_cell_length_c                   22.2153(7)
_cell_measurement_reflns_used    67367
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.9878
_cell_measurement_theta_min      3.3770
_cell_volume                     4922.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.935
_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  0.059
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            263202
_diffrn_reflns_theta_full        26.758
_diffrn_reflns_theta_max         30.065
_diffrn_reflns_theta_min         3.385
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2231.6
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.31
_refine_ls_extinction_coef       129(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0487
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         13519
_refine_ls_number_restraints     556
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.0148131
_refine_ls_shift/su_mean         0.0000689
_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:
0.140E+04 0.211E+04 0.111E+04 270.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1197
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1197
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                11032
_reflns_number_total             13520
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.46
_oxford_diffrn_Wilson_scale      0.17
_oxford_refine_ls_r_factor_ref   0.0757
_oxford_refine_ls_scale          2.432(14)
_oxford_reflns_number_all        13519
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c2dt11786j.txt
_cod_data_source_block           KOH
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 2/c '
_cod_database_code               7018184
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 29,X'S) H ( 291,X'S) H ( 293,X'S) H ( 292,X'S)
RIDE C ( 30,X'S) H ( 302,X'S) H ( 301,X'S) H ( 303,X'S)
RIDE C ( 31,X'S) H ( 313,X'S) H ( 312,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 322,X'S) H ( 323,X'S) H ( 321,X'S)
RIDE C ( 33,X'S) H ( 332,X'S) H ( 331,X'S) H ( 333,X'S)
RIDE C ( 34,X'S) H ( 343,X'S) H ( 341,X'S) H ( 342,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 ( 413,X'S) H ( 411,X'S) H ( 412,X'S)
RIDE C ( 42,X'S) H ( 422,X'S) H ( 423,X'S) H ( 421,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S)
RIDE C ( 47,X'S) H ( 471,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 56,X'S) H ( 561,X'S)
RIDE C ( 58,X'S) H ( 583,X'S) H ( 582,X'S) H ( 581,X'S)
RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) H ( 593,X'S)
RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S)
RIDE C ( 61,X'S) H ( 611,X'S) H ( 613,X'S) H ( 612,X'S)
RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S) H ( 623,X'S)
RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S) H ( 633,X'S)
RIDE C ( 66,X'S) H ( 661,X'S) H ( 662,X'S) H ( 663,X'S)
RIDE C ( 67,X'S) H ( 672,X'S) H ( 673,X'S) H ( 671,X'S)
RIDE C ( 68,X'S) H ( 682,X'S) H ( 683,X'S) H ( 681,X'S)
RIDE O ( 69,X'S) H ( 691,X'S)
RIDE O ( 71,X'S) H ( 711,X'S)
RIDE O ( 72,X'S) H ( 721,X'S)
RIDE C ( 73,X'S) H ( 731,X'S) H ( 733,X'S) H ( 732,X'S)
RIDE C ( 74,X'S) H ( 743,X'S) H ( 741,X'S) H ( 742,X'S)
RIDE O ( 75,X'S) H ( 751,X'S)
RIDE C ( 76,X'S) H ( 761,X'S) H ( 762,X'S) H ( 763,X'S)
RIDE O ( 77,X'S) H ( 771,X'S)
RIDE C ( 78,X'S) H ( 781,X'S) H ( 782,X'S) H ( 783,X'S)
RIDE O ( 79,X'S) H ( 791,X'S)
RIDE C ( 80,X'S) H ( 801,X'S) H ( 802,X'S) H ( 803,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
U(IJ)'S 0.0, 0.0010000 = C(31) TO C(27)
DISTANCE 1.550000 , 0.020000 = O(75) TO C(76)
DISTANCE 1.550000 , 0.020000 = O(77) TO C(78)
DISTANCE 1.550000 , 0.020000 = O(79) TO C(80)
U(IJ)'S 0.0, 0.0010000 = O(75) TO C(76)
U(IJ)'S 0.0, 0.0010000 = O(77) TO C(78)
U(IJ)'S 0.0, 0.0010000 = O(79) TO C(80)
U(IJ)'S 0.0, 0.0010000 = C(26) TO C(28)
U(IJ)'S 0.0, 0.0010000 = C(24) TO C(28)
U(IJ)'S 0.0, 0.0010000 = C(22) TO C(28)
U(IJ)'S 0.0, 0.0010000 = C(25) TO C(23)
U(IJ)'S 0.0, 0.0010000 = C(21) TO C(23)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE)
LIMIT 0.001000000 X
LIMIT 0.001000000 Y
LIMIT 0.001000000 Z
REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE)
END
;