Evidence for halogen bond covalency in acyclic and interlocked halogen-bonding receptor anion recognition.
Robinson, Sean W.; Mustoe, Chantal L.; White, Nicholas G.; Brown, Asha; Thompson, Amber L.; Kennepohl, Pierre; Beer, Paul D.; Journal of the American Chemical Society 137 (2015) 499–507; doi:10.1021/ja511648d

data_4123198
_publ_section_title
;
 Evidence for halogen bond covalency in acyclic and interlocked
 halogen-bonding receptor anion recognition.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              499
_journal_page_last               507
_journal_paper_doi               10.1021/ja511648d
_journal_volume                  137
_journal_year                    2015
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C34 H36 I2 N7 O6, C32 H38 N2 O9, 0.5(P O4)'
_chemical_formula_sum            'C66 H74 I2 N9 O17 P0.5'
_chemical_formula_weight         1534.66
_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     other
_cell_angle_alpha                78.599(3)
_cell_angle_beta                 89.672(3)
_cell_angle_gamma                66.939(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3757(4)
_cell_length_b                   16.0589(6)
_cell_length_c                   19.4107(7)
_cell_measurement_reflns_used    10478
_cell_measurement_temperature    0
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3748.6(2)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2010)'
_computing_data_collection       'Crystal Clear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2010)'
_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 0.879
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.098
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45435
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         26.376
_diffrn_reflns_theta_min         1.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1565
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as 
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.84
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         11532
_refine_ls_number_restraints     1063
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.0003503
_refine_ls_shift/su_mean         0.0000091
_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: 
 0.689E+04 0.116E+05 0.733E+04 0.317E+04 752. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3024
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.3024
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7734
_reflns_number_total             14253
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.87
_oxford_diffrn_Wilson_scale      0.14
_oxford_refine_ls_r_factor_ref   0.1033
_oxford_refine_ls_scale          3.48(7)
_oxford_reflns_number_all        11532
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            ja511648d_si_002.cif
_cod_data_source_block           9H2PO4
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 2935 2014-11-11 08:27:57Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4123193--4123198.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4123198