Bis-triazolium containing macrocycles, pseudorotaxanes and interlocked structures for anion recognition
White, Nicholas G.; Lovett, Henry G.; Beer, Paul D.; RSC Advances 4 (2014) 12133–; doi:10.1039/C4RA00615A

data_7235493
_publ_section_title
;
 Bis-triazolium containing macrocycles, pseudorotaxanes and interlocked
 structures for anion recognition
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              12133
_journal_paper_doi               10.1039/C4RA00615A
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        synthesized
_chemical_formula_moiety         '2(C31 H40 N6 O7)'
_chemical_formula_sum            'C62 H80 N12 O14'
_chemical_formula_weight         1217.39
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7515(2)
_cell_length_b                   65.1244(16)
_cell_length_c                   10.1151(3)
_cell_measurement_reflns_used    10973
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.1020
_cell_measurement_theta_min      1.8186
_cell_volume                     6423.7(3)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2011)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2011)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68889
_diffrn_reflns_av_R_equivalents  0.102
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       95
_diffrn_reflns_limit_k_min       -99
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            79874
_diffrn_reflns_theta_full        31.583
_diffrn_reflns_theta_max         33.245
_diffrn_reflns_theta_min         1.876
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis Pro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9502
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         8626
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.0005411
_refine_ls_shift/su_mean         0.0000386
_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: 
 62.1 100. 57.4 21.8 4.43 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1911
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.1911
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              99
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                7461
_reflns_number_total             12155
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.81
_oxford_diffrn_Wilson_scale      9.85
_oxford_refine_ls_r_factor_ref   0.0799
_oxford_refine_ls_scale          0.3509(5)
_oxford_reflns_number_all        8626
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c4ra00615a2.cif
_cod_data_source_block           propylmacrocycle4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_database_code               7235493