A hetero-phase growth method to control the crystal growth of β-antimony single crystals with high quality and large sizes
Zhao, Xuewen; Xu, Xuequan; Zhao, Rongzheng; Gu, Mengyue; Yang, Na; Huang, Lei; Fu, Chengcheng; Cheng, Yonghong; Zhang, Jinying; CrystEngComm  (2022) –; doi:10.1039/D2CE00743F

data_7245303
_publ_section_title
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 A hetero-phase growth method to control the crystal growth of \b-antimony
 single crystals with high quality and large sizes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00743F
_journal_year                    2022
_chemical_formula_moiety         0.167(Sb6)
_chemical_formula_sum            Sb
_chemical_formula_weight         121.75
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-03-21 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   4.2851(3)
_cell_length_b                   4.2851(3)
_cell_length_c                   11.3128(12)
_cell_measurement_reflns_used    469
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      5.41
_cell_volume                     179.90(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.967
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            457
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.210
_diffrn_reflns_theta_min         5.784
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.079
_exptl_absorpt_correction_T_max  0.0274
_exptl_absorpt_correction_T_min  0.0073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1536 before and 0.0774 after correction.
The Ratio of minimum to maximum transmission is 0.2664.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    6.743
_exptl_crystal_description       block
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.996
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.869
_refine_ls_extinction_coef       0.036(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5
_refine_ls_number_reflns         58
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0525
_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^)+(0.1000P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                58
_reflns_number_total             58
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00743f2.cif
_cod_data_source_block           mo_0408_20_0m
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7245303
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.177
_shelx_estimated_absorpt_t_min   0.096
_olex2_refinement_description
;
;
_shelx_res_checksum              24995
_olex2_submission_special_instructions 'No special instructions were received'