#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/43/7124319.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_7124319
loop_
_publ_author_name
'Müller, Matthias'
'Buchner, Magnus Richard'
_publ_section_title
;
 Preparation and Crystal Structures of the Beryllium Ammines [Be(NH3)4]X2
 (X = Br, I, CN, SCN, N3) and Be(NH3)2X’2 (X’ = Cl, Br, I).
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07712J
_journal_year                    2019
_chemical_formula_moiety         'C2 H12 Be1 N6'
_chemical_formula_sum            'C2 H12 Be N6'
_chemical_formula_weight         129.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-26 deposited with the CCDC.    2019-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1188(3)
_cell_length_b                   12.6103(6)
_cell_length_c                   6.9022(3)
_cell_measurement_reflns_used    6773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      158.34
_cell_measurement_theta_min      11.98
_cell_volume                     793.69(6)
_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 0.997
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8066
_diffrn_reflns_point_group_measured_fraction_full 0.836
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.681
_diffrn_reflns_theta_min         5.988
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1390
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0336
_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)+(0.0505P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.508
_reflns_Friedel_fraction_full    0.643
_reflns_Friedel_fraction_max     0.596
_reflns_number_gt                1129
_reflns_number_total             1390
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           FVAR2
_cod_database_code               7124319
_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'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.1423(2) 0.5436(2) 0.8334(4) 0.0421(7) Uani 0.16(3) 1 d P A 1
N1A N 0.1719(3) 0.6202(2) 0.7748(4) 0.0433(8) Uani 0.16(3) 1 d P A 1
N2A N 0.4948(3) 0.3345(2) 0.8715(4) 0.0435(8) Uani 0.60(4) 1 d P B 1
C2A C 0.4988(3) 0.3074(2) 0.7207(5) 0.0463(8) Uani 0.60(4) 1 d P B 1
C1B C 0.1719(3) 0.6202(2) 0.7748(4) 0.0433(8) Uani 0.84(3) 1 d P A 2
N1B N 0.1423(2) 0.5436(2) 0.8334(4) 0.0421(7) Uani 0.84(3) 1 d P A 2
C2B C 0.4948(3) 0.3345(2) 0.8715(4) 0.0435(8) Uani 0.40(4) 1 d P B 2
N2B N 0.4988(3) 0.3074(2) 0.7207(5) 0.0463(8) Uani 0.40(4) 1 d P B 2
Be1 Be 0.2507(3) 0.4158(2) 0.3127(6) 0.0273(5) Uani 1 1 d . . .
N3 N 0.1989(2) 0.36476(18) 0.5341(4) 0.0332(5) Uani 1 1 d . . .
H3A H 0.111(5) 0.324(3) 0.525(6) 0.055(10) Uiso 1 1 d . . .
H3B H 0.189(3) 0.415(3) 0.626(5) 0.046(9) Uiso 1 1 d . . .
H3C H 0.267(5) 0.316(3) 0.596(6) 0.075(12) Uiso 1 1 d . . .
N4 N 0.1840(3) 0.33828(17) 0.1298(3) 0.0344(5) Uani 1 1 d . . .
H4A H 0.222(6) 0.357(4) 0.001(8) 0.107(17) Uiso 1 1 d . . .
H4B H 0.079(6) 0.328(3) 0.124(6) 0.076(12) Uiso 1 1 d . . .
H4C H 0.222(5) 0.272(3) 0.136(6) 0.081(13) Uiso 1 1 d . . .
N6 N 0.1798(2) 0.54219(15) 0.2890(3) 0.0319(4) Uani 1 1 d . . .
H6A H 0.181(4) 0.572(3) 0.147(7) 0.076(12) Uiso 1 1 d . . .
H6B H 0.218(3) 0.592(3) 0.357(6) 0.051(9) Uiso 1 1 d . . .
H6C H 0.085(4) 0.541(3) 0.303(7) 0.073(11) Uiso 1 1 d . . .
N5 N 0.44016(19) 0.41708(17) 0.2999(4) 0.0302(4) Uani 1 1 d . . .
H5 H 0.481(4) 0.377(3) 0.395(6) 0.053(10) Uiso 1 1 d . . .
H5B H 0.483(3) 0.488(3) 0.292(7) 0.056(9) Uiso 1 1 d . . .
H5C H 0.470(4) 0.392(3) 0.172(6) 0.067(11) 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N4 Be1 N3 110.10(19)
N4 Be1 N6 108.9(2)
N3 Be1 N6 109.0(2)
N4 Be1 N5 108.8(2)
N3 Be1 N5 108.8(2)
N6 Be1 N5 111.10(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1A N1A 1.082(3)
N2A C2A 1.096(4)
C1B N1B 1.082(3)
C2B N2B 1.096(4)
Be1 N4 1.708(4)
Be1 N3 1.724(5)
Be1 N6 1.728(3)
Be1 N5 1.730(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
N3 H3A N2B^b 0.95(4) 2.37(4) 3.115(4) 135(3) 3_455 yes
N3 H3B N1B^b 0.90(4) 2.20(4) 3.102(4) 173(3) . yes
N3 H3C N2B^b 0.97(4) 2.29(5) 3.109(4) 142(3) . yes
N4 H4A N2A^a 0.98(6) 2.66(5) 3.349(4) 128(4) 1_554 yes
N4 H4A N1B^b 0.98(6) 2.73(5) 3.322(4) 119(3) 1_554 yes
N4 H4B N1A^a 0.97(5) 2.59(5) 3.436(3) 145(3) 2_564 yes
N4 H4C N1A^a 0.90(4) 2.35(4) 3.207(4) 158(4) 4_544 yes
N6 H6A N1A^a 1.05(5) 2.64(5) 3.684(4) 172(3) 1_554 yes
N6 H6A N1B^b 1.05(5) 2.22(4) 3.164(3) 148(3) 1_554 yes
N6 H6C N1B^b 0.87(4) 2.34(3) 3.145(3) 154(3) 2_564 yes
N5 H5 N2B^b 0.91(4) 2.42(4) 3.261(4) 155(3) . yes
N5 H5B N2A^a 0.97(3) 2.32(3) 3.226(3) 155(3) 2_664 yes
N5 H5B N2B^b 0.97(3) 2.63(3) 3.560(4) 159(3) 2_664 yes
N5 H5C N2A^a 0.98(4) 2.21(4) 3.174(4) 170(3) 1_554 yes
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168351036
