#------------------------------------------------------------------------------
#$Date: 2021-06-05 22:01:18 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266105 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/72/7707225.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_7707225
loop_
_publ_author_name
'Buchner, Magnus R.'
'Müller, Matthias'
_publ_section_title
;
 Ethylenediamine complexes of the beryllium halides and pseudo-halides.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7246
_journal_page_last               7255
_journal_paper_doi               10.1039/d1dt01154e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C6 H24 Be1 I2 N6'
_chemical_formula_sum            'C3 H12 Be0.5 I N3'
_chemical_formula_weight         221.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-07 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.712(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.5044(3)
_cell_length_b                   8.39210(10)
_cell_length_c                   15.9669(4)
_cell_measurement_reflns_used    33821
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      159.29
_cell_measurement_theta_min      11.28
_cell_volume                     1514.68(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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17984
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.776
_diffrn_reflns_theta_min         5.640
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    32.485
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_T_min  0.0000
_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    1.943
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.327
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       0.00062(9)
_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   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1012P)²+2.7351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1578
_reflns_number_total             1626
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01154e2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7707219--7707225.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C3 H12 Be0.50 I N3'
_cod_database_code               7707225
_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, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.10632(2) 0.77880(3) 0.65327(2) 0.0198(2) Uani 1 1 d . . . . .
N1 N 0.5601(3) 0.8443(4) 0.6777(2) 0.0193(7) Uani 1 1 d . . . . .
N2 N 0.4013(3) 0.6215(4) 0.6779(2) 0.0191(7) Uani 1 1 d . . . . .
N3 N 0.7503(4) 0.6757(5) 0.6107(2) 0.0228(7) Uani 1 1 d . . . . .
C1 C 0.4666(4) 0.8402(5) 0.5994(3) 0.0221(8) Uani 1 1 d . . . . .
C2 C 0.4188(4) 0.6700(5) 0.5911(2) 0.0205(8) Uani 1 1 d . . . . .
C3 C 0.7385(4) 0.6686(5) 0.5176(3) 0.0211(9) Uani 1 1 d . . . . .
Be1 Be 0.500000 0.7316(8) 0.750000 0.0189(15) Uani 1 2 d S T P . .
H1B H 0.632(6) 0.806(8) 0.666(4) 0.021(14) Uiso 1 1 d . . . . .
H1A H 0.579(4) 0.949(7) 0.691(3) 0.016(11) Uiso 1 1 d . . . . .
H2A H 0.412(5) 0.511(8) 0.682(4) 0.032(15) Uiso 1 1 d . . . . .
H2B H 0.336(7) 0.633(12) 0.684(5) 0.06(2) Uiso 1 1 d . . . . .
H1D H 0.498(5) 0.865(7) 0.545(4) 0.022(13) Uiso 1 1 d . . . . .
H1C H 0.403(4) 0.909(6) 0.608(3) 0.005(9) Uiso 1 1 d . . . . .
H2D H 0.480(5) 0.590(8) 0.574(4) 0.029(15) Uiso 1 1 d . . . . .
H2C H 0.352(6) 0.651(8) 0.548(4) 0.035(16) Uiso 1 1 d . . . . .
H3B H 0.832(7) 0.699(8) 0.638(5) 0.027(15) Uiso 1 1 d . . . . .
H3A H 0.735(5) 0.585(9) 0.630(4) 0.031(15) Uiso 1 1 d . . . . .
H3D H 0.792(6) 0.586(8) 0.500(4) 0.029(15) Uiso 1 1 d . . . . .
H3C H 0.657(5) 0.629(7) 0.493(3) 0.017(12) 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'
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
C1 N1 Be1 103.4(3) . . ?
C1 N1 H1B 110(4) . . ?
Be1 N1 H1B 115(4) . . ?
C1 N1 H1A 109(3) . . ?
Be1 N1 H1A 118(3) . . ?
H1B N1 H1A 102(5) . . ?
C2 N2 Be1 106.7(3) . . ?
C2 N2 H2A 108(4) . . ?
Be1 N2 H2A 115(4) . . ?
C2 N2 H2B 112(6) . . ?
Be1 N2 H2B 112(6) . . ?
H2A N2 H2B 103(8) . . ?
C3 N3 H3B 111(4) . . ?
C3 N3 H3A 111(4) . . ?
H3B N3 H3A 105(6) . . ?
N1 C1 C2 106.6(3) . . ?
N1 C1 H1D 113(3) . . ?
C2 C1 H1D 107(3) . . ?
N1 C1 H1C 109(3) . . ?
C2 C1 H1C 108(3) . . ?
H1D C1 H1C 113(4) . . ?
N2 C2 C1 106.4(3) . . ?
N2 C2 H2D 106(3) . . ?
C1 C2 H2D 112(3) . . ?
N2 C2 H2C 113(4) . . ?
C1 C2 H2C 117(4) . . ?
H2D C2 H2C 101(5) . . ?
N3 C3 C3 110.3(5) . 7_666 ?
N3 C3 H3D 112(3) . . ?
C3 C3 H3D 111(4) 7_666 . ?
N3 C3 H3C 108(3) . . ?
C3 C3 H3C 112(3) 7_666 . ?
H3D C3 H3C 104(5) . . ?
N2 Be1 N2 115.3(5) 2_656 . ?
N2 Be1 N1 98.20(17) 2_656 2_656 ?
N2 Be1 N1 116.22(18) . 2_656 ?
N2 Be1 N1 116.21(18) 2_656 . ?
N2 Be1 N1 98.20(17) . . ?
N1 Be1 N1 113.8(5) 2_656 . ?
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
N1 C1 1.491(5) . ?
N1 Be1 1.732(5) . ?
N1 H1B 0.94(7) . ?
N1 H1A 0.92(6) . ?
N2 C2 1.494(5) . ?
N2 Be1 1.727(5) . ?
N2 H2A 0.94(7) . ?
N2 H2B 0.79(8) . ?
N3 C3 1.469(6) . ?
N3 H3B 0.98(8) . ?
N3 H3A 0.86(7) . ?
C1 C2 1.528(5) . ?
C1 H1D 1.02(6) . ?
C1 H1C 0.96(5) . ?
C2 H2D 1.05(6) . ?
C2 H2C 0.95(7) . ?
C3 C3 1.518(8) 7_666 ?
C3 H3D 1.00(7) . ?
C3 H3C 1.00(6) . ?
