Stabilization of polyiodide chains via anion⋯anion interactions: experiment and theory
Lamberts, Kevin; Handels, Philipp; Englert, Ulli; Aubert, Emmanuel; Espinosa, Enrique; CrystEngComm 18 (2016) 3832–; doi:10.1039/C6CE00396F

data_7225042
_publ_section_title
;
 Stabilization of polyiodide chains via anion&#x22EF;anion interactions:
 experiment and theory
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3832
_journal_paper_doi               10.1039/C6CE00396F
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C9 H12 N O3, 2 I3, I2, 0.5(H2 O)'
_chemical_formula_sum            'C18 H25 I8 N2 O6.5'
_chemical_formula_weight         1388.60
_chemical_name_common
;
 L-tyrosiniumpolyiodide hydrate
;
_chemical_name_systematic        'compound 1'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2016-02-17 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.091(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8549(13)
_cell_length_b                   16.4789(18)
_cell_length_c                   17.3200(19)
_cell_measurement_reflns_used    9589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.47
_cell_volume                     3320.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 gonimeter with APEX CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'Incoatec microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45294
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.266
_diffrn_reflns_theta_min         1.198
_exptl_absorpt_coefficient_mu    7.507
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_description       plate
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.381
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         16441
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0800P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14914
_reflns_number_total             16441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00396f2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
          Adding full bibliography for 7225042.cif.

2017-03-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '4(C9 H12 N O3), I16, H2 O'
_cod_original_formula_sum        'C36 H50 I16 N4 O13'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2777.20
_cod_database_code               7225042
_shelx_estimated_absorpt_t_min   0.212
_shelx_estimated_absorpt_t_max   0.521
_shelxl_version_number           2013-2
_shelx_res_checksum              12389