A Raman Spectroscopic and Computational Study of New Aromatic Pyrimidine-Based Halogen Bond Acceptors
Hardin, A.E.S.; Ellington, T.L.; Nguyen, S.T.; Rheingold, A.L.; Tschumper, G.S.; Watkins, D.L.; Hammer, N.I.; Inorganics 7 (2019) 119–; doi:10.3390/inorganics7100119

data_1556444
_publ_section_title
;
 A Raman Spectroscopic and Computational Study of New Aromatic
 Pyrimidine-Based Halogen Bond Acceptors
;
_journal_name_full               Inorganics
_journal_page_first              119
_journal_paper_doi               10.3390/inorganics7100119
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         '2(C8 H3 I N2 O4), 2(C8 H6 N2 S)'
_chemical_formula_sum            'C32 H18 I2 N8 O8 S2'
_chemical_formula_weight         960.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 93.209(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2195(6)
_cell_length_b                   5.7344(4)
_cell_length_c                   32.1204(16)
_cell_measurement_reflns_used    6939
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.279
_cell_measurement_theta_min      2.539
_cell_volume                     1695.49(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            14426
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_min         2.267
_diffrn_source                   rotating-anode
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1977
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4232
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+2.5043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3944
_reflns_number_total             4232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dwat16_0m_a.cif
_cod_data_source_block           dwat16_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the built-in table derived from the CIF
Core dictionary named 'cif_core.dic' version 2.4.5 last updated on
2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1556444
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.570
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(S1')
Uanis(S1) = Uanis(C14')
3. Rigid body (RIGU) restrains
 C14', C16, C15, S1', C13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H16A)=Sof(H15A)=Sof(C14)=Sof(H14)=Sof(S1)=1-FVAR(1)
 Sof(S1')=Sof(H16)=Sof(H15)=Sof(C14')=Sof(H14')=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C9(H9), C4(H4), C6(H6), C16(H16), C16(H16A), C8(H8),
 C15(H15), C15(H15A), C14'(H14'), C14(H14)
;
_shelx_res_checksum              22725
_shelx_hkl_checksum              54995