Probing halogen bonds with solid-state NMR spectroscopy: observation and interpretation of J(77Se,31P) coupling in halogen-bonded PSe⋯I motifs
Viger-Gravel, Jasmine; Meyer, Julia E.; Korobkov, Ilia; Bryce, David L.; CrystEngComm 16 (2014) 7285–; doi:10.1039/C4CE00345D

data_7215248
_publ_section_title
;
 Probing halogen bonds with solid-state NMR spectroscopy: observation and
 interpretation of J(77Se,31P) coupling in halogen-bonded
 P&#xE001;Se&#x22EF;I motifs
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              7285
_journal_paper_doi               10.1039/C4CE00345D
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C24 H15 F3 I3 P Se'
_chemical_formula_weight         850.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.1691(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.1286(7)
_cell_length_b                   9.4276(3)
_cell_length_c                   23.3606(7)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.33
_cell_volume                     5085.9(3)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            77460
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.535
_diffrn_reflns_theta_min         1.764
_exptl_absorpt_coefficient_mu    5.214
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.625
_refine_diff_density_min         -2.108
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         15250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+6.4048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12901
_reflns_number_total             15250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce00345d2.cif
_cod_data_source_block           db115
_cod_depositor_comments
;Adding full bibliography for 7215248--7215249.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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 

2017-03-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C48 H30 F6 I6 P2 Se2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1701.98
_cod_database_code               7215248
_shelx_estimated_absorpt_t_min   0.393
_shelx_estimated_absorpt_t_max   0.550
_shelxl_version_number           2013-3
_shelx_res_checksum              64503