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_7235497
_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_compound_source        synthesized
_chemical_formula_moiety         'C36 H44 N6 O7, 0.5(C2 H3 N), H2 O, 2(N3)'
_chemical_formula_sum            'C37 H47.5 N12.5 O8'
_chemical_formula_weight         795.37
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                71.43(3)
_cell_angle_beta                 83.52(3)
_cell_angle_gamma                83.86(4)
_cell_formula_units_Z            2
_cell_length_a                   9.297(10)
_cell_length_b                   12.385(11)
_cell_length_c                   18.544(16)
_cell_measurement_reflns_used    3254
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      1.1
_cell_volume                     2005(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--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      150
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.157
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22114
_diffrn_reflns_theta_full        25.164
_diffrn_reflns_theta_max         30.688
_diffrn_reflns_theta_min         1.162
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         5086
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.1101
_refine_ls_shift/su_max          0.0007503
_refine_ls_shift/su_mean         0.0000321
_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: 
 55.1 86.5 52.5 21.0 4.72 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2467
_refine_ls_wR_factor_gt          0.2158
_refine_ls_wR_factor_ref         0.2467
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -14
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3336
_reflns_number_total             10447
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.89
_oxford_diffrn_Wilson_scale      12.11
_oxford_refine_ls_r_factor_ref   0.1618
_oxford_refine_ls_scale          0.3558(10)
_oxford_reflns_number_all        5086
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c4ra00615a2.cif
_cod_data_source_block           triazoliummacrocycle5N3
_cod_depositor_comments
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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 -1 '
_cod_database_code               7235497