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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/7/71/26/7712666.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_7712666
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_sum            'C6 H18 Be2 I4 P2'
_chemical_formula_weight         677.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-22 deposited with the CCDC.	2023-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.498(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9935(2)
_cell_length_b                   13.2512(2)
_cell_length_c                   10.5272(2)
_cell_measurement_reflns_used    28666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      79.16
_cell_measurement_theta_min      5.39
_cell_volume                     969.31(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      293(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17624
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.522
_diffrn_reflns_theta_min         5.388
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    51.819
_exptl_absorpt_correction_T_max  0.0036
_exptl_absorpt_correction_T_min  0.0002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.708
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         2067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0569
_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)+(0.1193P)²+3.4572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2012
_reflns_number_total             2067
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00713h2.cif
_cod_data_source_block           5_CCDC1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712666
_shelx_shelxl_version_number     2018/3
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
I1 I 0.72221(6) 0.58484(3) 0.50813(4) 0.0255(2) Uani 1 1 d . . . . .
C1 C 0.8304(12) 0.4442(8) 0.1818(8) 0.0375(17) Uani 1 1 d . . . . .
H1A H 0.886252 0.391094 0.136165 0.056 Uiso 1 1 calc R U . . .
H1B H 0.924616 0.469758 0.247355 0.056 Uiso 1 1 calc R U . . .
H1C H 0.788539 0.497647 0.123651 0.056 Uiso 1 1 calc R U . . .
P1 P 0.6243(2) 0.39495(13) 0.25484(16) 0.0226(4) Uani 1 1 d . . . . .
Be1 Be 0.4773(15) 0.5072(7) 0.3509(8) 0.0264(17) Uani 1 1 d . . . . .
I2 I 0.31117(6) 0.61811(3) 0.20913(4) 0.0298(2) Uani 1 1 d . . . . .
C2 C 0.4692(12) 0.3375(6) 0.1243(7) 0.0316(15) Uani 1 1 d . . . . .
H2A H 0.538266 0.285036 0.086234 0.047 Uiso 1 1 calc R U . . .
H2B H 0.429650 0.387850 0.061127 0.047 Uiso 1 1 calc R U . . .
H2C H 0.357794 0.309404 0.156601 0.047 Uiso 1 1 calc R U . . .
C3 C 0.7183(13) 0.2913(6) 0.3565(8) 0.0378(18) Uani 1 1 d . . . . .
H3A H 0.791717 0.246935 0.308722 0.057 Uiso 1 1 calc R U . . .
H3B H 0.613398 0.254727 0.386016 0.057 Uiso 1 1 calc R U . . .
H3C H 0.799492 0.317638 0.428593 0.057 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 0.0181 0.0091 '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 0.0038 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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 I1 Be1 78.5(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 . . ?
C3 P1 C2 105.9(4) . . ?
C3 P1 C1 105.5(4) . . ?
C2 P1 C1 105.2(4) . . ?
C3 P1 Be1 114.2(4) . . ?
C2 P1 Be1 111.9(4) . . ?
C1 P1 Be1 113.3(4) . . ?
P1 Be1 I2 111.8(4) . . ?
P1 Be1 I1 105.9(4) . . ?
I2 Be1 I1 115.4(4) . . ?
P1 Be1 I1 106.0(4) . 3_666 ?
I2 Be1 I1 115.1(4) . 3_666 ?
I1 Be1 I1 101.5(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
I1 Be1 2.467(10) . ?
I1 Be1 2.471(9) 3_666 ?
C1 P1 1.829(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
P1 C3 1.818(8) . ?
P1 C2 1.818(7) . ?
P1 Be1 2.128(10) . ?
Be1 I2 2.312(9) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2C I2 0.96 3.19 4.019(8) 145.2 2_545 yes
C3 H3A I2 0.96 3.28 4.134(8) 148.7 2_645 yes
