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#$Date: 2023-03-24 01:56:01 +0200 (Fri, 24 Mar 2023) $
#$Revision: 282029 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/26/7712664.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_7712664
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         'C6 H18 Be2 Cl4 P2'
_chemical_formula_sum            'C6 H18 Be2 Cl4 P2'
_chemical_formula_weight         311.96
_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     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                90
_cell_angle_beta                 100.175(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.2043(13)
_cell_length_b                   9.517(3)
_cell_length_c                   13.879(3)
_cell_measurement_reflns_used    1845
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.56
_cell_volume                     806.6(4)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area X-Red 1.65.2.0 (STOE, 2020)
;
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      ' 620 frames, detector distance = 120 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  0.1791
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10259
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.756
_diffrn_reflns_theta_min         2.608
_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    0.898
_exptl_absorpt_correction_T_max  0.5763
_exptl_absorpt_correction_T_min  0.3192
_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    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0918
_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/[σ²(Fo²)+(0.1732P)²+0.0617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2472
_refine_ls_wR_factor_ref         0.2604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1303
_reflns_number_total             1703
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00713h2.cif
_cod_data_source_block           1
_cod_original_cell_volume        806.6(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7712664
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Cl1 Cl 0.30455(19) 0.50330(10) 0.55887(9) 0.0489(4) Uani 1 1 d . . . . .
C1 C 0.0828(8) 0.1470(5) 0.4235(4) 0.0590(13) Uani 1 1 d . . . . .
H1A H -0.008037 0.206739 0.457632 0.088 Uiso 1 1 calc R U . . .
H1B H 0.150472 0.072880 0.467794 0.088 Uiso 1 1 calc R U . . .
H1C H -0.008581 0.104284 0.366159 0.088 Uiso 1 1 calc R U . . .
P1 P 0.2952(2) 0.25259(13) 0.38436(9) 0.0479(5) Uani 1 1 d . . . . .
Be1 Be 0.5003(9) 0.3566(7) 0.5041(4) 0.0489(14) Uani 1 1 d . . . . .
Cl2 Cl 0.6603(2) 0.22740(13) 0.59774(9) 0.0563(5) Uani 1 1 d . . . . .
C2 C 0.4430(9) 0.1328(6) 0.3197(4) 0.0621(13) Uani 1 1 d . . . . .
H2A H 0.547596 0.185382 0.288355 0.093 Uiso 1 1 calc R U . . .
H2B H 0.339819 0.082966 0.269624 0.093 Uiso 1 1 calc R U . . .
H2C H 0.522201 0.064720 0.365876 0.093 Uiso 1 1 calc R U . . .
C3 C 0.1522(10) 0.3712(6) 0.2919(4) 0.0652(14) Uani 1 1 d . . . . .
H3A H 0.259269 0.426166 0.263678 0.098 Uiso 1 1 calc R U . . .
H3B H 0.059132 0.434807 0.322075 0.098 Uiso 1 1 calc R U . . .
H3C H 0.061272 0.316598 0.240244 0.098 Uiso 1 1 calc R U . . .
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'
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'
Cl Cl 0.1484 0.1585 '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'
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
Be1 Cl1 Be1 81.8(3) . 3_666 ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 P1 C1 105.0(3) . . ?
C2 P1 C3 105.6(3) . . ?
C1 P1 C3 105.4(3) . . ?
C2 P1 Be1 113.2(2) . . ?
C1 P1 Be1 112.7(2) . . ?
C3 P1 Be1 114.1(3) . . ?
Cl2 Be1 Cl1 116.4(3) . . ?
Cl2 Be1 Cl1 114.8(3) . 3_666 ?
Cl1 Be1 Cl1 98.2(3) . 3_666 ?
Cl2 Be1 P1 113.0(3) . . ?
Cl1 Be1 P1 106.7(3) . . ?
Cl1 Be1 P1 106.1(3) 3_666 . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
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
Cl1 Be1 2.080(6) . ?
Cl1 Be1 2.093(6) 3_666 ?
C1 P1 1.815(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
P1 C2 1.800(5) . ?
P1 C3 1.818(5) . ?
P1 Be1 2.148(6) . ?
Be1 Cl2 1.931(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
