Highly Stable Organic Antimony Halide Crystals for X-ray Scintillation
He, Qingquan; Zhou, Chenkun; Xu, Liangjin; Lee, Sujin; Lin, Xinsong; Neu, Jennifer; Worku, Michael; Chaaban, Maya; Ma, Biwu; ACS Materials Letters 2 (2020) 633–638; doi:10.1021/acsmaterialslett.0c00133

data_4517652
_publ_section_title
;
 Highly Stable Organic Antimony Halide Crystals for X-ray Scintillation
;
_journal_issue                   6
_journal_name_full               'ACS Materials Letters'
_journal_page_first              633
_journal_page_last               638
_journal_paper_doi               10.1021/acsmaterialslett.0c00133
_journal_volume                  2
_journal_year                    2020
_chemical_formula_moiety         'Cl5 Sb, 2(C36 H30 N P2)'
_chemical_formula_sum            'C72 H60 Cl5 N2 P4 Sb'
_chemical_formula_weight         1376.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-17
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.6060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0421(2)
_cell_length_b                   24.1416(4)
_cell_length_c                   24.0743(4)
_cell_measurement_reflns_used    44683
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      32.7770
_cell_measurement_theta_min      2.0270
_cell_volume                     6417.22(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -42.00  32.00   0.50   19.00    --    6.83 -85.00  50.00  148
  2  \w    -23.00  39.00   0.50   19.00    --    6.83 -99.00 -30.00  124
  3  \w     -8.00  22.00   0.50   19.00    --   -7.92 -99.00-120.00   60
  4  \w    -23.00   8.00   0.50   19.00    --   -7.92 -99.00 -60.00   62
  5  \w    -42.00  17.00   0.50   19.00    --   -7.92 -85.00  50.00  118
  6  \w    -13.00  23.00   0.50   19.00    --   -7.92 -99.00 120.00   72
  7  \w    -33.00  21.00   0.50   19.00    --   -7.92  85.00 169.00  108
  8  \w    -67.00 -23.00   0.50   19.00    --    6.83 -19.00-150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0314754000
_diffrn_orient_matrix_UB_12      0.0239727000
_diffrn_orient_matrix_UB_13      -0.0091367000
_diffrn_orient_matrix_UB_21      0.0187698000
_diffrn_orient_matrix_UB_22      0.0141968000
_diffrn_orient_matrix_UB_23      0.0244262000
_diffrn_orient_matrix_UB_31      0.0527545000
_diffrn_orient_matrix_UB_32      0.0092812000
_diffrn_orient_matrix_UB_33      -0.0137546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            92625
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.601
_diffrn_reflns_theta_min         1.844
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2808
_exptl_crystal_preparation       'DCM as solvent'
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         19486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+0.8823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15668
_reflns_number_total             19486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz0c00133_si_002.cif
_cod_data_source_block           pacoa
_cod_depositor_comments
;Adding full bibliography for 4517652.cif.

 Adding full bibliography for 4517652.cif.
;
_cod_database_code               4517652
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C72H60P4N2SbCl5
_chemical_oxdiff_usercomment     '150K, Mo'
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2IA(H2IA), C3IA(H3IA), C4IA(H4IA), C5IA(H5IA), C6IA(H6IA), C2IB(H2IB),
 C3IB(H3IB), C4IB(H4IB), C5IB(H5IB), C6IB(H6IB), C2IC(H2IC), C3IC(H3IC),
 C4IC(H4IC), C5IC(H5IC), C6IC(H6IC), C2ID(H2ID), C3ID(H3ID), C4ID(H4ID),
 C5ID(H5ID), C6ID(H6ID), C2IE(H2IE), C3IE(H3IE), C4IE(H4IE), C5IE(H5IE),
 C6IE(H6IE), C2IF(H2IF), C3IF(H3IF), C4IF(H4IF), C5IF(H5IF), C6IF(H6IF),
 C2ZA(H2ZA), C3ZA(H3ZA), C4ZA(H4ZA), C5ZA(H5ZA), C6ZA(H6ZA), C2ZB(H2ZB),
 C3ZB(H3ZB), C4ZB(H4ZB), C5ZB(H5ZB), C6ZB(H6ZB), C2ZC(H2ZC), C3ZC(H3ZC),
 C4ZC(H4ZC), C5ZC(H5ZC), C6ZC(H6ZC), C2ZD(H2ZD), C3ZD(H3ZD), C4ZD(H4ZD),
 C5ZD(H5ZD), C6ZD(H6ZD), C2ZE(H2ZE), C3ZE(H3ZE), C4ZE(H4ZE), C5ZE(H5ZE),
 C6ZE(H6ZE), C2ZF(H2ZF), C3ZF(H3ZF), C4ZF(H4ZF), C5ZF(H5ZF), C6ZF(H6ZF)
;
_shelx_res_checksum              50300
_shelx_hkl_checksum              77652
_olex2_submission_original_sample_id PACOA
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.471
_oxdiff_exptl_absorpt_empirical_full_min 0.452