PbBe2B2O6: An Excellent Ultraviolet Nonlinear-Optical Crystal with Unprecedented π-π Interacting BeBO5 Group
Chen, Yi-Gang; Jiang, Xingxing; Yang, Yuanyu; Dai, Zhe; Lin, Zheshuai; Zhang, Xian-Ming; Chemical Communications  (2022) –; doi:10.1039/D2CC04631H

data_7130869
_publ_section_title
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 PbBe2B2O6: An Excellent Ultraviolet Nonlinear-Optical Crystal with
 Unprecedented \p-\p Interacting BeBO5 Group
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04631H
_journal_year                    2022
_chemical_formula_moiety         '0.5(B4 Be4 O12 Pb2)'
_chemical_formula_sum            'B2 Be2 O6 Pb'
_chemical_formula_weight         342.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_audit_creation_date             2022-10-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-10 deposited with the CCDC.	2022-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.737(2)
_cell_length_b                   4.7501(11)
_cell_length_c                   4.5368(11)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      3.80
_cell_volume                     231.39(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6469
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.442
_diffrn_reflns_theta_min         3.795
_exptl_absorpt_coefficient_mu    36.403
_exptl_absorpt_correction_T_max  0.1701
_exptl_absorpt_correction_T_min  0.0379
_exptl_absorpt_correction_type   'multi-scan and numerical'
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for empirical absorption correction (multi-scan).
wR2(int) was 0.1628 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.2228.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_coef       0.065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         730
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0173
_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^)+(0.0182P)^2^+1.0296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0425
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                730
_reflns_number_total             730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04631h2.cif
_cod_data_source_block           pbbe2b2o6
_cod_database_code               7130869
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
; 
SADABS-2016/2 - Bruker AXS area detector scaling and face absorption correction (numerical). 
Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10.
Mean and maximum errors in direction cosine check function =   0.000   0.000.
The mean error should not exceed 0.005, and is usually caused by matrix 
changes during data processing.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(3)
 0.46(3)
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
;
_shelx_res_checksum              48965
_shelx_hkl_checksum              75742
_olex2_submission_special_instructions 'No special instructions were received'