#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:37:18 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229635 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/77/7047763.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_7047763
loop_
_publ_author_name
'Buchner, Magnus R.'
'Müller, Matthias'
'Dankert, Fabian'
'Reuter, Kirsten'
'von Hänisch, Carsten'
_publ_section_title
;
 The coordination behaviour and reactivity of partially silicon based
 crown ethers towards beryllium chloride.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16393
_journal_page_last               16397
_journal_paper_doi               10.1039/c8dt03963a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'Be6C24H48ClO16 + CH2Cl2'
_chemical_formula_sum            'C25 H50 Be6 Cl6 O16'
_chemical_formula_weight         873.41
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-09 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.72(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.481(4)
_cell_length_b                   9.5492(19)
_cell_length_c                   21.762(4)
_cell_measurement_reflns_used    9356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.17
_cell_measurement_theta_min      4.21
_cell_volume                     3877.2(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  STOE_IPDS_2
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10000
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.324
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0525
_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)+(0.0669P)²+7.1537P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3201
_reflns_number_total             3895
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03963a2.cif
_cod_data_source_block           3_sq
_cod_depositor_comments
'Adding full bibliography for 7047763--7047764.cif.'
_cod_database_code               7047763
_shelx_shelxl_version_number     2014/7
_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
Cl1 Cl 0.64891(3) 0.55103(7) 0.40524(3) 0.03093(18) Uani 1 1 d . .
Cl2 Cl 0.62733(4) 0.76965(7) 0.65107(4) 0.03583(19) Uani 1 1 d . .
O1 O 0.66196(9) 0.5974(2) 0.54574(10) 0.0289(4) Uani 1 1 d . .
O2 O 0.63664(12) 0.0991(2) 0.49081(12) 0.0417(5) Uani 1 1 d . .
O3 O 0.58362(9) 0.46888(19) 0.61215(9) 0.0259(4) Uani 1 1 d . .
O4 O 0.57507(9) 0.39698(19) 0.49285(9) 0.0250(4) Uani 1 1 d . .
O5 O 0.56719(10) 0.1955(2) 0.57808(12) 0.0380(5) Uani 1 1 d . .
O6 O 0.46179(9) 0.34094(18) 0.53821(9) 0.0225(4) Uani 1 1 d . .
O7 O 0.72925(10) 0.5313(2) 0.65594(9) 0.0294(4) Uani 1 1 d . .
O8 O 0.67258(10) 0.3543(2) 0.72912(10) 0.0309(4) Uani 1 1 d . .
C1 C 0.76225(15) 0.5204(3) 0.72414(14) 0.0319(6) Uani 1 1 d . .
H1A H 0.7843 0.6111 0.7411 0.038 Uiso 1 1 calc R U
H1B H 0.8004 0.4485 0.7330 0.038 Uiso 1 1 calc R U
C2 C 0.59668(14) 0.3533(3) 0.71710(14) 0.0305(6) Uani 1 1 d . .
H2A H 0.5854 0.3714 0.7579 0.037 Uiso 1 1 calc R U
H2B H 0.5785 0.2587 0.7022 0.037 Uiso 1 1 calc R U
C3 C 0.55709(14) 0.4605(3) 0.66749(13) 0.0282(6) Uani 1 1 d . .
H3A H 0.5056 0.4358 0.6531 0.034 Uiso 1 1 calc R U
H3B H 0.5614 0.5538 0.6881 0.034 Uiso 1 1 calc R U
C4 C 0.55736(15) 0.2956(3) 0.44215(15) 0.0319(6) Uani 1 1 d . .
H4A H 0.5408 0.3451 0.4005 0.038 Uiso 1 1 calc R U
H4B H 0.5172 0.2370 0.4468 0.038 Uiso 1 1 calc R U
C5 C 0.77581(15) 0.5920(3) 0.62217(15) 0.0340(6) Uani 1 1 d . .
H5A H 0.8228 0.5438 0.6336 0.041 Uiso 1 1 calc R U
H5B H 0.7837 0.6928 0.6324 0.041 Uiso 1 1 calc R U
C6 C 0.70632(15) 0.4809(3) 0.75677(14) 0.0311(6) Uani 1 1 d . .
H6A H 0.7291 0.4677 0.8033 0.037 Uiso 1 1 calc R U
H6B H 0.6702 0.5565 0.7511 0.037 Uiso 1 1 calc R U
C7 C 0.67675(14) 0.1505(3) 0.55166(16) 0.0358(7) Uani 1 1 d . .
H7A H 0.6865 0.2515 0.5483 0.043 Uiso 1 1 calc R U
H7B H 0.7233 0.1010 0.5658 0.043 Uiso 1 1 calc R U
C8 C 0.63658(15) 0.1293(3) 0.60034(17) 0.0367(7) Uani 1 1 d . .
H8A H 0.6306 0.0279 0.6068 0.044 Uiso 1 1 calc R U
H8B H 0.6639 0.1704 0.6419 0.044 Uiso 1 1 calc R U
C9 C 0.73702(15) 0.5714(4) 0.55283(15) 0.0379(7) Uani 1 1 d . .
H9A H 0.7551 0.6375 0.5261 0.045 Uiso 1 1 calc R U
H9B H 0.7440 0.4747 0.5394 0.045 Uiso 1 1 calc R U
C10 C 0.50516(15) 0.1176(3) 0.57664(17) 0.0380(7) Uani 1 1 d . .
H10A H 0.5049 0.0943 0.6209 0.046 Uiso 1 1 calc R U
H10B H 0.5047 0.0290 0.5529 0.046 Uiso 1 1 calc R U
C11 C 0.61959(18) 0.2016(3) 0.44141(16) 0.0392(7) Uani 1 1 d . .
H11A H 0.6083 0.1534 0.3994 0.047 Uiso 1 1 calc R U
H11B H 0.6624 0.2607 0.4453 0.047 Uiso 1 1 calc R U
C12 C 0.44232(18) 0.2004(3) 0.5453(3) 0.0625(13) Uani 1 1 d . .
H12A H 0.4185 0.1601 0.5025 0.075 Uiso 1 1 calc R U
H12B H 0.4080 0.1975 0.5711 0.075 Uiso 1 1 calc R U
Be1 Be 0.60422(17) 0.5501(4) 0.47971(16) 0.0237(6) Uani 1 1 d . .
Be2 Be 0.54698(17) 0.3649(3) 0.55343(18) 0.0247(7) Uani 1 1 d . .
Be3 Be 0.64393(19) 0.5840(4) 0.61321(18) 0.0300(7) Uani 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 0.0033 0.0016 '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 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
C9 O1 Be3 111.6(2) . .
C9 O1 Be1 118.1(2) . .
Be3 O1 Be1 120.7(2) . .
C7 O2 C11 114.5(2) . .
C3 O3 Be3 117.5(2) . .
C3 O3 Be2 116.4(2) . .
Be3 O3 Be2 126.0(2) . .
C4 O4 Be2 116.3(2) . .
C4 O4 Be1 119.4(2) . .
Be2 O4 Be1 122.6(2) . .
C10 O5 C8 119.3(2) . .
C10 O5 Be2 111.8(2) . .
C8 O5 Be2 128.8(2) . .
C12 O6 Be2 113.9(2) . .
C12 O6 Be1 114.7(2) . 5_666
Be2 O6 Be1 131.3(2) . 5_666
C1 O7 C5 113.2(2) . .
C1 O7 Be3 130.5(2) . .
C5 O7 Be3 104.9(2) . .
C6 O8 C2 114.3(2) . .
O7 C1 C6 109.5(2) . .
O7 C1 H1A 109.8 . .
C6 C1 H1A 109.8 . .
O7 C1 H1B 109.8 . .
C6 C1 H1B 109.8 . .
H1A C1 H1B 108.2 . .
O8 C2 C3 114.3(2) . .
O8 C2 H2A 108.7 . .
C3 C2 H2A 108.7 . .
O8 C2 H2B 108.7 . .
C3 C2 H2B 108.7 . .
H2A C2 H2B 107.6 . .
O3 C3 C2 113.5(2) . .
O3 C3 H3A 108.9 . .
C2 C3 H3A 108.9 . .
O3 C3 H3B 108.9 . .
C2 C3 H3B 108.9 . .
H3A C3 H3B 107.7 . .
O4 C4 C11 113.1(2) . .
O4 C4 H4A 109.0 . .
C11 C4 H4A 109.0 . .
O4 C4 H4B 109.0 . .
C11 C4 H4B 109.0 . .
H4A C4 H4B 107.8 . .
O7 C5 C9 104.6(2) . .
O7 C5 H5A 110.8 . .
C9 C5 H5A 110.8 . .
O7 C5 H5B 110.8 . .
C9 C5 H5B 110.8 . .
H5A C5 H5B 108.9 . .
O8 C6 C1 108.8(2) . .
O8 C6 H6A 109.9 . .
C1 C6 H6A 109.9 . .
O8 C6 H6B 109.9 . .
C1 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
O2 C7 C8 110.7(3) . .
O2 C7 H7A 109.5 . .
C8 C7 H7A 109.5 . .
O2 C7 H7B 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
O5 C8 C7 109.4(2) . .
O5 C8 H8A 109.8 . .
C7 C8 H8A 109.8 . .
O5 C8 H8B 109.8 . .
C7 C8 H8B 109.8 . .
H8A C8 H8B 108.2 . .
O1 C9 C5 106.7(2) . .
O1 C9 H9A 110.4 . .
C5 C9 H9A 110.4 . .
O1 C9 H9B 110.4 . .
C5 C9 H9B 110.4 . .
H9A C9 H9B 108.6 . .
O5 C10 C12 108.9(2) . .
O5 C10 H10A 109.9 . .
C12 C10 H10A 109.9 . .
O5 C10 H10B 109.9 . .
C12 C10 H10B 109.9 . .
H10A C10 H10B 108.3 . .
O2 C11 C4 114.5(3) . .
O2 C11 H11A 108.6 . .
C4 C11 H11A 108.6 . .
O2 C11 H11B 108.6 . .
C4 C11 H11B 108.6 . .
H11A C11 H11B 107.6 . .
O6 C12 C10 110.6(3) . .
O6 C12 H12A 109.5 . .
C10 C12 H12A 109.5 . .
O6 C12 H12B 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 108.1 . .
O6 Be1 O1 109.7(2) 5_666 .
O6 Be1 O4 109.2(2) 5_666 .
O1 Be1 O4 106.5(2) . .
O6 Be1 Cl1 107.25(18) 5_666 .
O1 Be1 Cl1 110.93(18) . .
O4 Be1 Cl1 113.16(19) . .
O4 Be2 O6 115.8(2) . .
O4 Be2 O3 111.0(2) . .
O6 Be2 O3 116.4(2) . .
O4 Be2 O5 109.7(2) . .
O6 Be2 O5 93.46(19) . .
O3 Be2 O5 108.9(2) . .
O3 Be3 O1 113.1(2) . .
O3 Be3 O7 113.3(2) . .
O1 Be3 O7 94.9(2) . .
O3 Be3 Cl2 113.9(2) . .
O1 Be3 Cl2 113.9(2) . .
O7 Be3 Cl2 106.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Be1 2.049(3) .
Cl2 Be3 2.020(4) .
O1 C9 1.447(3) .
O1 Be3 1.610(4) .
O1 Be1 1.614(4) .
O2 C7 1.417(4) .
O2 C11 1.421(4) .
O3 C3 1.443(3) .
O3 Be3 1.604(4) .
O3 Be2 1.613(4) .
O4 C4 1.433(3) .
O4 Be2 1.596(4) .
O4 Be1 1.623(4) .
O5 C10 1.411(3) .
O5 C8 1.444(3) .
O5 Be2 1.715(4) .
O6 C12 1.415(3) .
O6 Be2 1.613(4) .
O6 Be1 1.613(4) 5_666
O7 C1 1.441(3) .
O7 C5 1.443(3) .
O7 Be3 1.730(4) .
O8 C6 1.424(3) .
O8 C2 1.426(3) .
C1 C6 1.509(4) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.526(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C11 1.512(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C9 1.494(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.501(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C12 1.452(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
Be1 O6 1.613(4) 5_666
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
C1 H1A O8 0.99 2.49 3.474(4) 172.0 4_656
C3 H3A Cl1 0.99 2.91 3.869(3) 162.5 5_666
C3 H3A O6 0.99 2.56 3.108(3) 114.5 .
C3 H3B Cl2 0.99 2.67 3.316(3) 122.9 .
C6 H6B Cl2 0.99 2.92 3.637(3) 130.0 .
C7 H7A O4 0.99 2.57 3.105(3) 114.1 .
C7 H7B Cl1 0.99 2.79 3.779(3) 174.8 7_656
C8 H8A Cl2 0.99 2.65 3.627(3) 167.4 1_545
C8 H8B O8 0.99 2.56 3.440(4) 148.7 .
C11 H11B Cl1 0.99 2.90 3.512(3) 121.2 .
C12 H12B Cl1 0.99 2.75 3.325(4) 117.1 5_666
