A ferrocene redox-active triazolium macrocycle that binds and senses chloride.
White, Nicholas G.; Beer, Paul D.; Beilstein journal of organic chemistry 8 (2012) 246–252; doi:10.3762/bjoc.8.25

data_4029714
_publ_section_title
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 A ferrocene redox-active triazolium macrocycle that binds and senses
 chloride.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              246
_journal_page_last               252
_journal_paper_doi               10.3762/bjoc.8.25
_journal_volume                  8
_journal_year                    2012
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C26 H26 Fe1 N6'
_chemical_formula_sum            'C26 H26 Fe N6'
_chemical_formula_weight         478.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 92.6441(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7117(2)
_cell_length_b                   11.9571(2)
_cell_length_c                   32.2561(6)
_cell_measurement_reflns_used    18186
_cell_measurement_temperature    100
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     4512.27(14)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device       synchrotron
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            47035
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         30.241
_diffrn_reflns_theta_min         1.687
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0444
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         7393
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.0008335
_refine_ls_shift/su_mean         0.0000221
_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: 
 0.324E+04 0.469E+04 0.284E+04 0.119E+04 133. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1525
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1525
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                7068
_reflns_number_total             13163
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.54
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0673
_oxford_refine_ls_scale          4.14(7)
_oxford_reflns_number_all        7393
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            1860-5397-8-25-S2.cif
_cod_data_source_block           3
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/Beilstein/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C26 H26 Fe1 N6'
_cod_database_code               4029714
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 463,X'S) H   ( 464,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  59,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) H   ( 602,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) 
RIDE C   ( 166,X'S) H   (1661,X'S) H   (1662,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 662,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 1.52, 0.02 = C(46) TO C(66), C(66) TO C(65) 
CONT C(46) TO C(166), C(166) TO C(65) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00200 = C(19) TO C(20) 
VIBR .0, 0.00500 = C(20) TO C(18) 
VIBR .0, 0.00200 = C(20) TO C(21) 
VIBR .0, 0.00500 = C(22) TO C(20) 
VIBR .0, 0.00200 = C(46) TO C(66) 
VIBR .0, 0.00500 = C(66) TO C(44) 
VIBR .0, 0.00200 = C(65) TO C(66) 
VIBR .0, 0.00500 = C(66) TO C(64) 
VIBR .0, 0.00200 = C(46) TO C(166) 
VIBR .0, 0.00500 = C(166) TO C(44) 
VIBR .0, 0.00200 = C(65) TO C(166) 
VIBR .0, 0.00500 = C(166) TO C(64) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = C(19) TO C(20) 
U(IJ) .0, 0.04000 = C(20) TO C(21) 
U(IJ) .0, 0.04000 = C(46) TO C(66) 
U(IJ) .0, 0.04000 = C(65) TO C(66) 
U(IJ) .0, 0.04000 = C(46) TO C(166) 
U(IJ) .0, 0.04000 = C(65) TO C(166) 
REM   THERMSIM   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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