#------------------------------------------------------------------------------
#$Date: 2020-07-06 05:12:39 +0200 (lun 06 de jul de 2020) $
#$Revision: 253915 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/41/7704172.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_7704172
loop_
_publ_author_name
'Buchner, Magnus R.'
'Müller, Matthias'
'Spang, Nils'
_publ_section_title
;
 Probing the electronic boundaries between trigonal and tetrahedral
 coordination at beryllium.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7708
_journal_page_last               7712
_journal_paper_doi               10.1039/d0dt01442g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C7 H17 Be Cl4 N'
_chemical_formula_weight         266.02
_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
;
2020-04-01 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.947(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0572(3)
_cell_length_b                   8.7404(2)
_cell_length_c                   13.0930(3)
_cell_measurement_reflns_used    22788
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      152.30
_cell_measurement_theta_min      10.12
_cell_volume                     1264.63(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15955
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.694
_diffrn_reflns_theta_min         5.326
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    8.157
_exptl_absorpt_correction_T_max  0.0351
_exptl_absorpt_correction_T_min  0.0094
_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    1.397
_exptl_crystal_description       column
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.665
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0405
_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)+(0.0688P)²+2.3780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2423
_reflns_number_total             2596
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01442g2.cif
_cod_data_source_block           2_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7704167--7704172.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704172
_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
Cl1 Cl 0.58541(8) 0.72487(10) 0.36444(6) 0.0417(2) Uani 1 1 d . . . . .
N1 N 0.4992(2) 0.4761(3) 0.26188(17) 0.0224(5) Uani 1 1 d . . . . .
Be1 Be 0.8791(3) 0.5343(4) 0.5167(3) 0.0255(7) Uani 1 1 d . . . . .
C1 C 0.4749(3) 0.6433(3) 0.2814(2) 0.0248(6) Uani 1 1 d . . . . .
H1A H 0.394394 0.654324 0.311510 0.030 Uiso 1 1 calc R U . . .
H1AB H 0.473169 0.699276 0.215630 0.030 Uiso 1 1 calc R U . . .
Cl2 Cl 0.97279(6) 0.50648(8) 0.38116(5) 0.02636(19) Uani 1 1 d . . . . .
C2 C 0.6257(3) 0.4508(3) 0.2225(2) 0.0276(6) Uani 1 1 d . . . . .
H2A H 0.631051 0.345005 0.196045 0.033 Uiso 1 1 calc R U . . .
H2AB H 0.685065 0.460652 0.280405 0.033 Uiso 1 1 calc R U . . .
Cl3 Cl 0.82228(6) 0.74654(7) 0.53204(5) 0.02833(19) Uani 1 1 d . . . . .
C3 C 0.6615(3) 0.5643(4) 0.1363(2) 0.0285(6) Uani 1 1 d . . . . .
H3A H 0.739754 0.534066 0.109740 0.043 Uiso 1 1 calc R U . . .
H3B H 0.667361 0.668123 0.164211 0.043 Uiso 1 1 calc R U . . .
H3C H 0.599672 0.561739 0.080831 0.043 Uiso 1 1 calc R U . . .
C4 C 0.4071(3) 0.4225(3) 0.1801(2) 0.0253(6) Uani 1 1 d . . . . .
H4A H 0.424596 0.314573 0.163103 0.030 Uiso 1 1 calc R U . . .
H4AB H 0.417515 0.484046 0.117577 0.030 Uiso 1 1 calc R U . . .
Cl4 Cl 0.75656(6) 0.37210(7) 0.52636(5) 0.02607(19) Uani 1 1 d . . . . .
C5 C 0.2740(3) 0.4345(3) 0.2111(2) 0.0266(6) Uani 1 1 d . . . . .
H5A H 0.220707 0.401329 0.153961 0.040 Uiso 1 1 calc R U . . .
H5B H 0.255525 0.540802 0.228494 0.040 Uiso 1 1 calc R U . . .
H5C H 0.261181 0.368899 0.270465 0.040 Uiso 1 1 calc R U . . .
C7 C 0.4989(2) 0.2085(3) 0.35236(18) 0.0182(5) Uani 1 1 d . . . . .
H7A H 0.486515 0.161284 0.419098 0.027 Uiso 1 1 calc R U . . .
H7B H 0.579969 0.183247 0.329567 0.027 Uiso 1 1 calc R U . . .
H7C H 0.438115 0.169626 0.302645 0.027 Uiso 1 1 calc R U . . .
C6 C 0.4858(3) 0.3891(3) 0.3617(2) 0.0247(6) Uani 1 1 d . . . . .
H6A H 0.405416 0.412663 0.388887 0.030 Uiso 1 1 calc R U . . .
H6AB H 0.547763 0.426806 0.411981 0.030 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
C1 N1 C2 111.6(2) . . ?
C1 N1 C6 108.3(2) . . ?
C2 N1 C6 109.6(2) . . ?
C1 N1 C4 107.3(2) . . ?
C2 N1 C4 108.5(2) . . ?
C6 N1 C4 111.5(2) . . ?
Cl3 Be1 Cl4 116.66(19) . . ?
Cl3 Be1 Cl2 111.30(17) . . ?
Cl4 Be1 Cl2 109.36(18) . . ?
Cl3 Be1 Cl2 109.75(17) . 3_766 ?
Cl4 Be1 Cl2 111.04(18) . 3_766 ?
Cl2 Be1 Cl2 96.99(15) . 3_766 ?
N1 C1 Cl1 111.9(2) . . ?
Be1 Cl2 Be1 83.01(15) . 3_766 ?
N1 C2 C3 114.2(2) . . ?
N1 C4 C5 114.5(2) . . ?
N1 C6 C7 114.7(2) . . ?
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 C1 1.759(3) . ?
N1 C1 1.509(3) . ?
N1 C2 1.523(4) . ?
N1 C6 1.524(3) . ?
N1 C4 1.526(3) . ?
Be1 Cl3 1.971(4) . ?
Be1 Cl4 1.968(4) . ?
Be1 Cl2 2.099(4) . ?
Be1 Cl2 2.109(4) 3_766 ?
C2 C3 1.563(4) . ?
C4 C5 1.543(4) . ?
C7 C6 1.591(4) . ?
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
C1 H1A Cl4 0.99 2.75 3.652(3) 151.1 3_666 yes
C1 H1AB Cl3 0.99 2.92 3.749(3) 142.2 4_575 yes
C3 H3B Cl1 0.98 2.85 3.431(3) 119.1 . yes
C4 H4A Cl2 0.99 2.99 3.963(3) 168.9 2_645 yes
C4 H4AB Cl3 0.99 2.80 3.589(3) 137.4 4_575 yes
C5 H5A Cl4 0.98 2.95 3.611(3) 125.6 4_565 yes
C5 H5C Cl3 0.98 2.95 3.898(3) 162.3 3_666 yes
C6 H6A Cl4 0.99 2.85 3.735(3) 149.5 3_666 yes
C6 H6AB Cl4 0.99 2.75 3.632(3) 148.5 . yes
