#------------------------------------------------------------------------------
#$Date: 2023-03-24 01:56:01 +0200 (Fri, 24 Mar 2023) $
#$Revision: 282029 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/26/7712667.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_7712667
loop_
_publ_author_name
'Buchner, Magnus Richard'
'Cocic, Dusan'
'Ivlev, Sergei'
'Spang, Nils'
'Müller, Matthias'
'Puchta, Ralph'
_publ_section_title
;
 Ligand exchange at tetra-coordinated beryllium centres
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00713H
_journal_year                    2023
_chemical_formula_moiety         'C36 H66 Be2 Br4 P2'
_chemical_formula_sum            'C36 H66 Be2 Br4 P2'
_chemical_formula_weight         898.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2023-03-22 deposited with the CCDC.	2023-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                95.17(3)
_cell_angle_beta                 110.54(3)
_cell_angle_gamma                90.53(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5773(19)
_cell_length_b                   10.134(2)
_cell_length_c                   10.971(2)
_cell_measurement_reflns_used    16258
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.80
_cell_measurement_theta_min      3.82
_cell_volume                     992.1(4)
_computing_cell_refinement       'X-Area v1.81 (Stoe, 2018)'
_computing_data_collection       'X-Area v1.81 (Stoe, 2018)'
_computing_data_reduction        'X-Area v1.81 (Stoe, 2018)'
_computing_molecular_graphics    'Diamond v4.5.2 (Brandenburg, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      ' 310 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16237
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.219
_diffrn_reflns_theta_min         1.992
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.161
_exptl_absorpt_correction_T_max  0.5439
_exptl_absorpt_correction_T_min  0.1904
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0348
_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)+(0.0420P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3850
_reflns_number_total             5339
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00713h2.cif
_cod_data_source_block           1_a_CCDC1
_cod_database_code               7712667
_shelx_shelxl_version_number     2019/1
_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.
;
_shelx_estimated_absorpt_t_min   0.490
_shelx_estimated_absorpt_t_max   0.574
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Br01 Br 0.34106(3) 0.40527(3) 0.45744(3) 0.02619(8) Uani 1 1 d . . . . .
Br02 Br 0.59973(3) 0.39759(3) 0.78448(3) 0.03230(9) Uani 1 1 d . . . . .
P003 P 0.40054(8) 0.69542(7) 0.69819(7) 0.02277(15) Uani 1 1 d . . . . .
C004 C 0.3440(3) 0.8151(3) 0.5732(3) 0.0241(5) Uani 1 1 d . . . . .
H004 H 0.433264 0.830501 0.548183 0.029 Uiso 1 1 calc R U . . .
C005 C 0.3042(4) 0.9524(3) 0.6189(3) 0.0325(6) Uani 1 1 d . . . . .
H00A H 0.215569 0.943097 0.644546 0.039 Uiso 1 1 calc R U . . .
H00B H 0.388174 0.990554 0.696903 0.039 Uiso 1 1 calc R U . . .
C006 C 0.5301(3) 0.7941(3) 0.8440(2) 0.0249(6) Uani 1 1 d . . . . .
H006 H 0.473869 0.870273 0.864917 0.030 Uiso 1 1 calc R U . . .
C007 C 0.5869(3) 0.7195(3) 0.9662(3) 0.0295(6) Uani 1 1 d . . . . .
H00C H 0.501251 0.681415 0.983917 0.035 Uiso 1 1 calc R U . . .
H00D H 0.647966 0.645648 0.951358 0.035 Uiso 1 1 calc R U . . .
C008 C 0.7592(3) 0.9461(3) 0.9338(3) 0.0312(6) Uani 1 1 d . . . . .
H00E H 0.846863 0.980177 0.916354 0.037 Uiso 1 1 calc R U . . .
H00F H 0.700771 1.022699 0.946606 0.037 Uiso 1 1 calc R U . . .
C009 C 0.6632(3) 0.8534(3) 0.8166(3) 0.0275(6) Uani 1 1 d . . . . .
H00G H 0.724061 0.781125 0.798233 0.033 Uiso 1 1 calc R U . . .
H00H H 0.626294 0.903074 0.738503 0.033 Uiso 1 1 calc R U . . .
C00A C 0.1940(3) 0.7568(3) 0.8282(3) 0.0297(6) Uani 1 1 d . . . . .
H00I H 0.271114 0.757544 0.916432 0.036 Uiso 1 1 calc R U . . .
H00J H 0.194544 0.846368 0.798902 0.036 Uiso 1 1 calc R U . . .
C00B C 0.8124(3) 0.8758(3) 1.0580(3) 0.0325(6) Uani 1 1 d . . . . .
H00K H 0.868104 0.940190 1.133267 0.039 Uiso 1 1 calc R U . . .
H00L H 0.880891 0.805936 1.049484 0.039 Uiso 1 1 calc R U . . .
C00C C 0.2717(4) 1.0462(3) 0.5130(3) 0.0349(7) Uani 1 1 d . . . . .
H00M H 0.363713 1.063231 0.494166 0.042 Uiso 1 1 calc R U . . .
H00N H 0.241489 1.131807 0.544832 0.042 Uiso 1 1 calc R U . . .
C00D C 0.2195(3) 0.7607(3) 0.4472(3) 0.0331(6) Uani 1 1 d . . . . .
H00O H 0.247431 0.674080 0.415162 0.040 Uiso 1 1 calc R U . . .
H00P H 0.126924 0.746007 0.465750 0.040 Uiso 1 1 calc R U . . .
C00E C 0.6806(3) 0.8134(3) 1.0831(3) 0.0309(6) Uani 1 1 d . . . . .
H00Q H 0.718020 0.764122 1.161330 0.037 Uiso 1 1 calc R U . . .
H00R H 0.617626 0.884199 1.100665 0.037 Uiso 1 1 calc R U . . .
C00F C 0.2308(3) 0.6555(3) 0.7338(3) 0.0289(6) Uani 1 1 d . . . . .
H00S H 0.146231 0.656230 0.648609 0.035 Uiso 1 1 calc R U . . .
C00G C 0.1902(4) 0.8544(3) 0.3416(3) 0.0359(7) Uani 1 1 d . . . . .
H00T H 0.107810 0.816634 0.262240 0.043 Uiso 1 1 calc R U . . .
H00U H 0.280524 0.864609 0.318522 0.043 Uiso 1 1 calc R U . . .
C00H C 0.1490(3) 0.9897(3) 0.3882(3) 0.0314(6) Uani 1 1 d . . . . .
H00V H 0.134566 1.050749 0.319618 0.038 Uiso 1 1 calc R U . . .
H00W H 0.054075 0.980879 0.404356 0.038 Uiso 1 1 calc R U . . .
C00I C 0.0315(3) 0.5871(3) 0.8725(3) 0.0382(7) Uani 1 1 d . . . . .
H00X H -0.071767 0.567593 0.867920 0.046 Uiso 1 1 calc R U . . .
H00Y H 0.099177 0.582179 0.963855 0.046 Uiso 1 1 calc R U . . .
C00J C 0.2255(4) 0.5155(3) 0.7743(3) 0.0368(7) Uani 1 1 d . . . . .
H00Z H 0.244445 0.450316 0.709668 0.044 Uiso 1 1 calc R U . . .
H010 H 0.304193 0.508864 0.860558 0.044 Uiso 1 1 calc R U . . .
C00K C 0.0729(3) 0.4843(3) 0.7820(3) 0.0380(7) Uani 1 1 d . . . . .
H011 H -0.003774 0.480537 0.693198 0.046 Uiso 1 1 calc R U . . .
H012 H 0.073004 0.395927 0.813845 0.046 Uiso 1 1 calc R U . . .
C00L C 0.0432(4) 0.7240(3) 0.8345(3) 0.0381(7) Uani 1 1 d . . . . .
H013 H 0.023607 0.789172 0.898701 0.046 Uiso 1 1 calc R U . . .
H014 H -0.034329 0.731860 0.747867 0.046 Uiso 1 1 calc R U . . .
Be0M Be 0.5024(4) 0.5205(4) 0.6360(3) 0.0269(7) 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
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Be0M Br01 Be0M 82.47(13) . 2_666 ?
C006 P003 C00F 107.24(12) . . ?
C006 P003 C004 103.75(12) . . ?
C00F P003 C004 105.75(13) . . ?
C006 P003 Be0M 112.89(14) . . ?
C00F P003 Be0M 113.83(13) . . ?
C004 P003 Be0M 112.60(13) . . ?
C00D C004 C005 109.2(3) . . ?
C00D C004 P003 113.55(19) . . ?
C005 C004 P003 116.02(18) . . ?
C00D C004 H004 105.7 . . ?
C005 C004 H004 105.7 . . ?
P003 C004 H004 105.7 . . ?
C00C C005 C004 111.9(2) . . ?
C00C C005 H00A 109.2 . . ?
C004 C005 H00A 109.2 . . ?
C00C C005 H00B 109.2 . . ?
C004 C005 H00B 109.2 . . ?
H00A C005 H00B 107.9 . . ?
C007 C006 C009 109.7(2) . . ?
C007 C006 P003 114.41(19) . . ?
C009 C006 P003 111.48(17) . . ?
C007 C006 H006 107.0 . . ?
C009 C006 H006 107.0 . . ?
P003 C006 H006 107.0 . . ?
C00E C007 C006 109.9(2) . . ?
C00E C007 H00C 109.7 . . ?
C006 C007 H00C 109.7 . . ?
C00E C007 H00D 109.7 . . ?
C006 C007 H00D 109.7 . . ?
H00C C007 H00D 108.2 . . ?
C00B C008 C009 111.6(2) . . ?
C00B C008 H00E 109.3 . . ?
C009 C008 H00E 109.3 . . ?
C00B C008 H00F 109.3 . . ?
C009 C008 H00F 109.3 . . ?
H00E C008 H00F 108.0 . . ?
C008 C009 C006 110.2(2) . . ?
C008 C009 H00G 109.6 . . ?
C006 C009 H00G 109.6 . . ?
C008 C009 H00H 109.6 . . ?
C006 C009 H00H 109.6 . . ?
H00G C009 H00H 108.1 . . ?
C00L C00A C00F 110.7(2) . . ?
C00L C00A H00I 109.5 . . ?
C00F C00A H00I 109.5 . . ?
C00L C00A H00J 109.5 . . ?
C00F C00A H00J 109.5 . . ?
H00I C00A H00J 108.1 . . ?
C008 C00B C00E 110.8(2) . . ?
C008 C00B H00K 109.5 . . ?
C00E C00B H00K 109.5 . . ?
C008 C00B H00L 109.5 . . ?
C00E C00B H00L 109.5 . . ?
H00K C00B H00L 108.1 . . ?
C005 C00C C00H 111.7(2) . . ?
C005 C00C H00M 109.3 . . ?
C00H C00C H00M 109.3 . . ?
C005 C00C H00N 109.3 . . ?
C00H C00C H00N 109.3 . . ?
H00M C00C H00N 107.9 . . ?
C00G C00D C004 111.9(2) . . ?
C00G C00D H00O 109.2 . . ?
C004 C00D H00O 109.2 . . ?
C00G C00D H00P 109.2 . . ?
C004 C00D H00P 109.2 . . ?
H00O C00D H00P 107.9 . . ?
C007 C00E C00B 111.1(2) . . ?
C007 C00E H00Q 109.4 . . ?
C00B C00E H00Q 109.4 . . ?
C007 C00E H00R 109.4 . . ?
C00B C00E H00R 109.4 . . ?
H00Q C00E H00R 108.0 . . ?
C00A C00F C00J 110.6(2) . . ?
C00A C00F P003 115.59(19) . . ?
C00J C00F P003 113.6(2) . . ?
C00A C00F H00S 105.3 . . ?
C00J C00F H00S 105.3 . . ?
P003 C00F H00S 105.3 . . ?
C00D C00G C00H 110.8(2) . . ?
C00D C00G H00T 109.5 . . ?
C00H C00G H00T 109.5 . . ?
C00D C00G H00U 109.5 . . ?
C00H C00G H00U 109.5 . . ?
H00T C00G H00U 108.1 . . ?
C00C C00H C00G 110.0(3) . . ?
C00C C00H H00V 109.7 . . ?
C00G C00H H00V 109.7 . . ?
C00C C00H H00W 109.7 . . ?
C00G C00H H00W 109.7 . . ?
H00V C00H H00W 108.2 . . ?
C00L C00I C00K 110.7(2) . . ?
C00L C00I H00X 109.5 . . ?
C00K C00I H00X 109.5 . . ?
C00L C00I H00Y 109.5 . . ?
C00K C00I H00Y 109.5 . . ?
H00X C00I H00Y 108.1 . . ?
C00K C00J C00F 109.9(3) . . ?
C00K C00J H00Z 109.7 . . ?
C00F C00J H00Z 109.7 . . ?
C00K C00J H010 109.7 . . ?
C00F C00J H010 109.7 . . ?
H00Z C00J H010 108.2 . . ?
C00I C00K C00J 112.4(2) . . ?
C00I C00K H011 109.1 . . ?
C00J C00K H011 109.1 . . ?
C00I C00K H012 109.1 . . ?
C00J C00K H012 109.1 . . ?
H011 C00K H012 107.9 . . ?
C00I C00L C00A 112.7(3) . . ?
C00I C00L H013 109.1 . . ?
C00A C00L H013 109.1 . . ?
C00I C00L H014 109.1 . . ?
C00A C00L H014 109.1 . . ?
H013 C00L H014 107.8 . . ?
Br02 Be0M P003 114.08(15) . . ?
Br02 Be0M Br01 111.34(16) . . ?
P003 Be0M Br01 111.42(17) . . ?
Br02 Be0M Br01 114.36(17) . 2_666 ?
P003 Be0M Br01 106.89(16) . 2_666 ?
Br01 Be0M Br01 97.52(13) . 2_666 ?
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
Br01 Be0M 2.240(4) . ?
Br01 Be0M 2.250(3) 2_666 ?
Br02 Be0M 2.096(4) . ?
P003 C006 1.843(3) . ?
P003 C00F 1.850(3) . ?
P003 C004 1.853(3) . ?
P003 Be0M 2.200(4) . ?
C004 C00D 1.527(4) . ?
C004 C005 1.533(4) . ?
C004 H004 1.0000 . ?
C005 C00C 1.516(4) . ?
C005 H00A 0.9900 . ?
C005 H00B 0.9900 . ?
C006 C007 1.531(4) . ?
C006 C009 1.539(3) . ?
C006 H006 1.0000 . ?
C007 C00E 1.521(4) . ?
C007 H00C 0.9900 . ?
C007 H00D 0.9900 . ?
C008 C00B 1.522(4) . ?
C008 C009 1.523(4) . ?
C008 H00E 0.9900 . ?
C008 H00F 0.9900 . ?
C009 H00G 0.9900 . ?
C009 H00H 0.9900 . ?
C00A C00L 1.505(4) . ?
C00A C00F 1.523(4) . ?
C00A H00I 0.9900 . ?
C00A H00J 0.9900 . ?
C00B C00E 1.526(4) . ?
C00B H00K 0.9900 . ?
C00B H00L 0.9900 . ?
C00C C00H 1.517(4) . ?
C00C H00M 0.9900 . ?
C00C H00N 0.9900 . ?
C00D C00G 1.515(4) . ?
C00D H00O 0.9900 . ?
C00D H00P 0.9900 . ?
C00E H00Q 0.9900 . ?
C00E H00R 0.9900 . ?
C00F C00J 1.530(4) . ?
C00F H00S 1.0000 . ?
C00G C00H 1.524(4) . ?
C00G H00T 0.9900 . ?
C00G H00U 0.9900 . ?
C00H H00V 0.9900 . ?
C00H H00W 0.9900 . ?
C00I C00L 1.498(4) . ?
C00I C00K 1.525(4) . ?
C00I H00X 0.9900 . ?
C00I H00Y 0.9900 . ?
C00J C00K 1.526(4) . ?
C00J H00Z 0.9900 . ?
C00J H010 0.9900 . ?
C00K H011 0.9900 . ?
C00K H012 0.9900 . ?
C00L H013 0.9900 . ?
C00L H014 0.9900 . ?
