#------------------------------------------------------------------------------
#$Date: 2020-07-06 06:12:39 +0300 (Mon, 06 Jul 2020) $
#$Revision: 253915 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/41/7704168.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_7704168
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_moiety         'C12 H30 Be2 Br4 N2'
_chemical_formula_sum            'C6 H15 Be Br2 N'
_chemical_formula_weight         270.02
_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   difmap
_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                 93.991(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8122(3)
_cell_length_b                   9.8904(3)
_cell_length_c                   13.0159(5)
_cell_measurement_reflns_used    18876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      160.18
_cell_measurement_theta_min      6.81
_cell_volume                     1003.24(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0145
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9510
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.892
_diffrn_reflns_theta_min         5.623
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    9.704
_exptl_absorpt_correction_T_max  0.1105
_exptl_absorpt_correction_T_min  0.0274
_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    1.788
_exptl_crystal_description       rod
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00055(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0187
_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)+(0.0312P)²+0.6501P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2107
_reflns_number_total             2138
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01442g2.cif
_cod_data_source_block           3_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7704167--7704172.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7704168
_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
Br1 Br 0.30463(2) 0.22484(2) 0.45985(2) 0.02358(8) Uani 1 1 d . . . . .
Br2 Br 0.41103(2) 0.52212(2) 0.61349(2) 0.02162(8) Uani 1 1 d . . . . .
N1 N 0.6782(2) 0.27022(15) 0.59084(12) 0.0200(3) Uani 1 1 d . . . . .
C1 C 0.7219(3) 0.1353(2) 0.54489(15) 0.0232(4) Uani 1 1 d . . . . .
C2 C 0.7905(3) 0.1419(2) 0.43866(16) 0.0275(4) Uani 1 1 d . . . . .
C3 C 0.8324(2) 0.3634(2) 0.59646(16) 0.0237(4) Uani 1 1 d . . . . .
C4 C 0.9888(3) 0.3150(2) 0.66296(17) 0.0283(4) Uani 1 1 d . . . . .
C5 C 0.6342(3) 0.2442(2) 0.70043(15) 0.0238(4) Uani 1 1 d . . . . .
C6 C 0.4697(3) 0.1660(2) 0.71398(16) 0.0285(4) Uani 1 1 d . . . . .
Be1 Be 0.5063(3) 0.3496(2) 0.51999(18) 0.0211(4) Uani 1 1 d . . . . .
H1A H 0.800(4) 0.093(3) 0.590(2) 0.034(7) Uiso 1 1 d . . . . .
H1B H 0.615(3) 0.079(3) 0.5427(19) 0.023(6) Uiso 1 1 d . . . . .
H2B H 0.902(4) 0.185(3) 0.438(2) 0.048(8) Uiso 1 1 d . . . . .
H2C H 0.806(4) 0.049(3) 0.413(2) 0.036(7) Uiso 1 1 d . . . . .
H2A H 0.713(3) 0.185(3) 0.388(2) 0.029(6) Uiso 1 1 d . . . . .
H3B H 0.866(3) 0.373(3) 0.527(2) 0.027(6) Uiso 1 1 d . . . . .
H3A H 0.797(3) 0.449(3) 0.6216(19) 0.018(5) Uiso 1 1 d . . . . .
H4C H 1.028(3) 0.228(3) 0.642(2) 0.030(7) Uiso 1 1 d . . . . .
H4B H 1.081(4) 0.379(3) 0.653(2) 0.039(7) Uiso 1 1 d . . . . .
H4A H 0.968(4) 0.308(3) 0.734(2) 0.038(7) Uiso 1 1 d . . . . .
H5B H 0.726(4) 0.196(3) 0.732(2) 0.033(7) Uiso 1 1 d . . . . .
H5A H 0.633(3) 0.331(3) 0.7363(19) 0.024(6) Uiso 1 1 d . . . . .
H6A H 0.458(4) 0.150(3) 0.786(2) 0.047(8) Uiso 1 1 d . . . . .
H6B H 0.371(4) 0.212(3) 0.685(2) 0.041(8) Uiso 1 1 d . . . . .
H6C H 0.471(3) 0.082(3) 0.681(2) 0.034(7) Uiso 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 0.0181 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'
Br Br -0.6763 1.2805 '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 Br2 Be1 83.58(9) . 3_666 ?
C1 N1 C5 107.19(14) . . ?
C1 N1 C3 110.84(15) . . ?
C5 N1 C3 106.86(14) . . ?
C1 N1 Be1 111.82(14) . . ?
C5 N1 Be1 110.79(14) . . ?
C3 N1 Be1 109.21(14) . . ?
N1 C1 C2 115.23(16) . . ?
N1 C3 C4 116.08(16) . . ?
N1 C5 C6 116.43(16) . . ?
N1 Be1 Br1 117.17(13) . . ?
N1 Be1 Br2 108.88(12) . . ?
Br1 Be1 Br2 112.17(11) . . ?
N1 Be1 Br2 113.65(13) . 3_666 ?
Br1 Be1 Br2 106.65(10) . 3_666 ?
Br2 Be1 Br2 96.42(9) . 3_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
Br1 Be1 2.108(2) . ?
Br2 Be1 2.252(2) . ?
Br2 Be1 2.281(2) 3_666 ?
N1 C1 1.511(2) . ?
N1 C5 1.512(2) . ?
N1 C3 1.515(2) . ?
N1 Be1 1.760(3) . ?
C1 C2 1.519(3) . ?
C3 C4 1.525(3) . ?
C5 C6 1.521(3) . ?
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 H1B Br1 1.00(3) 2.96(2) 3.483(2) 113.4(17) . yes
C1 H1B Br1 1.00(3) 3.07(3) 3.569(2) 112.0(16) 3_656 yes
C2 H2B Br1 0.97(3) 3.16(3) 4.090(2) 160(2) 1_655 yes
C2 H2A Br2 0.96(3) 3.06(3) 3.719(2) 127.3(19) 3_666 yes
C3 H3B Br2 0.96(3) 2.93(2) 3.412(2) 112.7(17) 3_666 yes
C3 H3A Br2 0.96(3) 3.09(2) 3.667(2) 120.3(16) . yes
C4 H4B Br2 0.97(3) 3.02(3) 3.973(2) 168(2) 1_655 yes
C5 H5B Br1 0.94(3) 3.09(3) 3.5555(19) 113(2) 4_666 yes
C6 H6B Br1 0.95(3) 2.95(3) 3.514(2) 120(2) . yes
