#------------------------------------------------------------------------------
#$Date: 2022-10-15 00:59:02 +0300 (Sat, 15 Oct 2022) $
#$Revision: 278592 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/08/7130869.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7130869
loop_
_publ_author_name
'Chen, Yi-Gang'
'Jiang, Xingxing'
'Yang, Yuanyu'
'Dai, Zhe'
'Lin, Zheshuai'
'Zhang, Xian-Ming'
_publ_section_title
;
 PbBe2B2O6: An Excellent Ultraviolet Nonlinear-Optical Crystal with
 Unprecedented π-π Interacting BeBO5 Group
;
_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 λ/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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0182P)²+1.0296P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            d2cc04631h2.cif
_cod_data_source_block           pbbe2b2o6
_cod_database_code               7130869
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.0000 -0.82387(5) -0.14392(15) 0.01651(17) Uani 1 2 d S T P . .
O1 O 0.1363(5) -0.9042(11) -0.635(8) 0.0429(18) Uani 1 1 d . U . . .
O2 O -0.1327(6) -1.2016(12) -0.2800(13) 0.0180(11) Uani 1 1 d . . . . .
Be1 Be -0.2489(11) -1.3208(16) -0.207(2) 0.017(2) Uani 1 1 d . . . . .
O3 O -0.2911(6) -1.6194(13) -0.2370(12) 0.0172(10) Uani 1 1 d . U . . .
B1 B 0.1581(9) -1.1617(15) -0.5750(18) 0.0155(18) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 65.9(8) 3 . ?
O2 Pb1 O1 90.2(3) . . ?
O2 Pb1 O1 90.2(3) 3 3 ?
O2 Pb1 O1 49.5(3) 3 . ?
O2 Pb1 O1 49.5(3) . 3 ?
O2 Pb1 O2 73.8(3) 3 . ?
Be1 O1 Pb1 118.3(12) 4_534 . ?
B1 O1 Pb1 93.4(16) . . ?
B1 O1 Be1 121.5(7) . 4_534 ?
Be1 O2 Pb1 140.7(5) . . ?
B1 O2 Pb1 105.5(4) 3 . ?
B1 O2 Be1 96.2(7) 3 . ?
O1 Be1 O3 92.1(12) 4_435 2_425 ?
O1 Be1 B1 105.8(11) 4_435 3 ?
O2 Be1 O1 116.3(6) . 4_435 ?
O2 Be1 O3 96.1(6) . 2_425 ?
O2 Be1 O3 128.9(8) . . ?
O2 Be1 B1 41.3(4) . 3 ?
O3 Be1 O1 113.8(7) . 4_435 ?
O3 Be1 O3 91.4(5) . 2_425 ?
O3 Be1 B1 114.5(6) . 3 ?
B1 Be1 O3 137.5(6) 3 2_425 ?
Be1 O3 Be1 98.7(5) . 2_424 ?
B1 O3 Be1 119.7(5) 4_425 2_424 ?
B1 O3 Be1 141.5(7) 4_425 . ?
O1 B1 O2 107.6(16) . 3 ?
O1 B1 Be1 127.4(14) . 3 ?
O1 B1 O3 132.8(17) . 4_524 ?
O2 B1 Be1 42.5(5) 3 3 ?
O2 B1 O3 119.3(6) 3 4_524 ?
O3 B1 Be1 88.2(5) 4_524 3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.69(3) . ?
Pb1 O1 2.69(3) 3 ?
Pb1 O2 2.373(6) . ?
Pb1 O2 2.373(6) 3 ?
O1 Be1 1.664(14) 4_534 ?
O1 B1 1.275(12) . ?
O2 Be1 1.409(13) . ?
O2 B1 1.379(10) 3 ?
Be1 O1 1.664(14) 4_435 ?
Be1 O3 2.194(11) 2_425 ?
Be1 O3 1.495(10) . ?
Be1 B1 2.076(13) 3 ?
O3 Be1 2.194(11) 2_424 ?
O3 B1 1.385(10) 4_425 ?
B1 O2 1.379(10) 3 ?
B1 Be1 2.075(13) 3 ?
B1 O3 1.385(10) 4_524 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54(3)
2 0.46(3)
