#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:37:18 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229635 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/77/7047764.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_7047764
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         'C36 H40 Be6 Cl4 O14, 2(C6 H6)'
_chemical_formula_sum            'C48 H52 Be6 Cl4 O14'
_chemical_formula_weight         1048.75
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-09-09 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                108.235(2)
_cell_angle_beta                 103.883(2)
_cell_angle_gamma                106.623(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8872(5)
_cell_length_b                   12.0013(6)
_cell_length_c                   12.2122(6)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.91
_cell_measurement_theta_min      2.36
_cell_volume                     1229.35(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.909
_diffrn_reflns_theta_max         24.909
_diffrn_reflns_theta_min         2.306
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9341
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0833 before and 0.0482 after correction. The Ratio of minimum to maximum transmission is 0.9341. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0402
_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)+(0.0414P)²+1.6165P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3716
_reflns_number_total             4297
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03963a2.cif
_cod_data_source_block           062_0m
_cod_depositor_comments
'Adding full bibliography for 7047763--7047764.cif.'
_cod_database_code               7047764
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C17(H17A,H17B), C18(H18A,H18B), C1(H1A,H1B), C10(H10A,H10B),
 C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C7(H7), C12(H12), C4(H4), C6(H6), C13(H13), C21(H21), C14(H14),
 C5(H5), C24(H24), C20(H20), C22(H22), C19(H19), C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Cl2 Cl 0.76564(6) 0.84228(5) 1.02112(5) 0.02080(15) Uani 1 1 d .
Cl1 Cl 0.13881(6) 0.49038(5) 0.73846(5) 0.02354(15) Uani 1 1 d .
O1 O 0.51439(16) 0.32475(13) 0.95849(13) 0.0136(3) Uani 1 1 d .
O3 O 0.64319(16) 0.55823(13) 0.95408(13) 0.0145(3) Uani 1 1 d .
O4 O 0.47794(16) 0.63369(13) 0.81596(13) 0.0150(3) Uani 1 1 d .
O7 O 0.38293(16) 0.38747(13) 0.77723(13) 0.0143(3) Uani 1 1 d .
O5 O 0.34975(17) 0.48182(14) 0.59732(13) 0.0180(3) Uani 1 1 d .
O6 O 0.37418(18) 0.25589(15) 0.54005(14) 0.0207(4) Uani 1 1 d .
O2 O 0.66399(17) 0.35730(15) 0.82176(14) 0.0187(3) Uani 1 1 d .
C16 C 0.2516(2) 0.3844(2) 0.48183(19) 0.0173(5) Uani 1 1 d .
C11 C 0.2630(3) 0.2670(2) 0.4565(2) 0.0182(5) Uani 1 1 d .
C8 C 0.6069(2) 0.2588(2) 0.9529(2) 0.0173(5) Uani 1 1 d .
C15 C 0.1493(3) 0.4023(2) 0.3965(2) 0.0202(5) Uani 1 1 d .
H15 H 0.1407 0.4824 0.4156 0.024 Uiso 1 1 calc R
C3 C 0.6944(3) 0.2782(2) 0.8817(2) 0.0194(5) Uani 1 1 d .
C9 C 0.2719(3) 0.2591(2) 0.7044(2) 0.0194(5) Uani 1 1 d .
H9A H 0.1745 0.2614 0.6623 0.023 Uiso 1 1 calc R
H9B H 0.2556 0.2152 0.7594 0.023 Uiso 1 1 calc R
C7 C 0.6199(3) 0.1791(2) 1.0120(2) 0.0213(5) Uani 1 1 d .
H7 H 0.5614 0.1647 1.0613 0.026 Uiso 1 1 calc R
C12 C 0.1715(3) 0.1666(2) 0.3427(2) 0.0228(5) Uani 1 1 d .
H12 H 0.1778 0.0857 0.3246 0.027 Uiso 1 1 calc R
C17 C 0.4011(3) 0.6138(2) 0.6102(2) 0.0215(5) Uani 1 1 d .
H17A H 0.3201 0.6466 0.6112 0.026 Uiso 1 1 calc R
H17B H 0.4363 0.6223 0.5427 0.026 Uiso 1 1 calc R
C4 C 0.7959(3) 0.2217(2) 0.8666(2) 0.0230(5) Uani 1 1 d .
H4 H 0.8547 0.2369 0.8177 0.028 Uiso 1 1 calc R
C18 C 0.5300(3) 0.6816(2) 0.7333(2) 0.0196(5) Uani 1 1 d .
H18A H 0.6200 0.6640 0.7254 0.023 Uiso 1 1 calc R
H18B H 0.5578 0.7748 0.7643 0.023 Uiso 1 1 calc R
C6 C 0.7208(3) 0.1206(2) 0.9973(2) 0.0240(5) Uani 1 1 d .
H6 H 0.7301 0.0650 1.0368 0.029 Uiso 1 1 calc R
C1 C 0.7971(2) 0.5697(2) 0.9733(2) 0.0224(5) Uani 1 1 d .
H1A H 0.8368 0.5493 1.0438 0.027 Uiso 1 1 calc R
H1B H 0.8630 0.6575 0.9906 0.027 Uiso 1 1 calc R
C13 C 0.0708(3) 0.1841(2) 0.2554(2) 0.0236(5) Uani 1 1 d .
H13 H 0.0096 0.1157 0.1770 0.028 Uiso 1 1 calc R
C10 C 0.3230(3) 0.1858(2) 0.6092(2) 0.0220(5) Uani 1 1 d .
H10A H 0.4064 0.1663 0.6512 0.026 Uiso 1 1 calc R
H10B H 0.2380 0.1039 0.5513 0.026 Uiso 1 1 calc R
C21 C 0.5882(3) 0.0564(2) 0.3090(2) 0.0299(6) Uani 1 1 d .
H21 H 0.5133 0.0056 0.2286 0.036 Uiso 1 1 calc R
C2 C 0.7920(3) 0.4760(2) 0.8555(2) 0.0263(5) Uani 1 1 d .
H2A H 0.7768 0.5075 0.7895 0.032 Uiso 1 1 calc R
H2B H 0.8876 0.4622 0.8684 0.032 Uiso 1 1 calc R
C14 C 0.0594(3) 0.3016(2) 0.2826(2) 0.0234(5) Uani 1 1 d .
H14 H -0.0104 0.3131 0.2229 0.028 Uiso 1 1 calc R
C5 C 0.8085(3) 0.1408(2) 0.9267(2) 0.0263(6) Uani 1 1 d .
H5 H 0.8770 0.0999 0.9190 0.032 Uiso 1 1 calc R
C24 C 0.8052(3) 0.2058(3) 0.5421(2) 0.0363(7) Uani 1 1 d .
H24 H 0.8800 0.2567 0.6226 0.044 Uiso 1 1 calc R
C20 C 0.5450(3) 0.0895(3) 0.4077(3) 0.0353(6) Uani 1 1 d .
H20 H 0.4408 0.0609 0.3972 0.042 Uiso 1 1 calc R
C22 C 0.7369(3) 0.0949(3) 0.3234(3) 0.0406(7) Uani 1 1 d .
H22 H 0.7659 0.0702 0.2536 0.049 Uiso 1 1 calc R
C19 C 0.6575(3) 0.1673(3) 0.5264(3) 0.0395(7) Uani 1 1 d .
H19 H 0.6284 0.1927 0.5960 0.047 Uiso 1 1 calc R
C23 C 0.8476(3) 0.1713(3) 0.4418(3) 0.0434(8) Uani 1 1 d .
H23 H 0.9518 0.1991 0.4524 0.052 Uiso 1 1 calc R
Be2 Be 0.5908(3) 0.6748(3) 0.9551(3) 0.0150(6) Uani 1 1 d .
Be3 Be 0.3432(3) 0.4958(3) 0.7438(3) 0.0161(6) Uani 1 1 d .
Be1 Be 0.5326(3) 0.4117(3) 0.8797(3) 0.0160(6) 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'
Cl Cl 0.1484 0.1585 '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'
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
C8 O1 Be2 123.63(16) . 2_667
C8 O1 Be1 111.81(17) . .
Be1 O1 Be2 124.35(16) . 2_667
C1 O3 Be2 122.58(17) . .
C1 O3 Be1 109.03(16) . .
Be1 O3 Be2 123.70(17) . .
C18 O4 Be2 121.14(17) . .
C18 O4 Be3 112.12(16) . .
Be3 O4 Be2 119.86(16) . .
C9 O7 Be3 115.72(16) . .
C9 O7 Be1 119.37(16) . .
Be1 O7 Be3 124.90(17) . .
C16 O5 C17 119.00(16) . .
C16 O5 Be3 127.68(16) . .
C17 O5 Be3 103.27(15) . .
C11 O6 C10 115.90(17) . .
C3 O2 C2 115.72(17) . .
C3 O2 Be1 105.02(16) . .
C2 O2 Be1 103.48(16) . .
C11 C16 O5 116.00(18) . .
C15 C16 O5 122.8(2) . .
C15 C16 C11 121.2(2) . .
O6 C11 C16 119.24(19) . .
O6 C11 C12 121.3(2) . .
C12 C11 C16 119.2(2) . .
O1 C8 C3 114.75(19) . .
O1 C8 C7 125.8(2) . .
C7 C8 C3 119.5(2) . .
C16 C15 H15 120.4 . .
C16 C15 C14 119.1(2) . .
C14 C15 H15 120.5 . .
C8 C3 O2 113.33(19) . .
C4 C3 O2 123.4(2) . .
C4 C3 C8 123.2(2) . .
O7 C9 H9A 109.4 . .
O7 C9 H9B 109.4 . .
O7 C9 C10 110.95(19) . .
H9A C9 H9B 108.0 . .
C10 C9 H9A 109.4 . .
C10 C9 H9B 109.4 . .
C8 C7 H7 120.9 . .
C8 C7 C6 118.2(2) . .
C6 C7 H7 120.9 . .
C11 C12 H12 119.9 . .
C13 C12 C11 120.1(2) . .
C13 C12 H12 119.9 . .
O5 C17 H17A 111.4 . .
O5 C17 H17B 111.4 . .
O5 C17 C18 102.05(17) . .
H17A C17 H17B 109.2 . .
C18 C17 H17A 111.4 . .
C18 C17 H17B 111.4 . .
C3 C4 H4 121.5 . .
C3 C4 C5 117.0(2) . .
C5 C4 H4 121.5 . .
O4 C18 C17 106.50(18) . .
O4 C18 H18A 110.4 . .
O4 C18 H18B 110.4 . .
C17 C18 H18A 110.4 . .
C17 C18 H18B 110.4 . .
H18A C18 H18B 108.6 . .
C7 C6 H6 119.0 . .
C5 C6 C7 122.1(2) . .
C5 C6 H6 119.0 . .
O3 C1 H1A 110.5 . .
O3 C1 H1B 110.5 . .
O3 C1 C2 105.97(18) . .
H1A C1 H1B 108.7 . .
C2 C1 H1A 110.5 . .
C2 C1 H1B 110.5 . .
C12 C13 H13 120.0 . .
C12 C13 C14 120.0(2) . .
C14 C13 H13 120.0 . .
O6 C10 C9 112.12(18) . .
O6 C10 H10A 109.2 . .
O6 C10 H10B 109.2 . .
C9 C10 H10A 109.2 . .
C9 C10 H10B 109.2 . .
H10A C10 H10B 107.9 . .
C20 C21 H21 119.5 . .
C20 C21 C22 121.0(2) . .
C22 C21 H21 119.5 . .
O2 C2 C1 105.86(18) . .
O2 C2 H2A 110.6 . .
O2 C2 H2B 110.6 . .
C1 C2 H2A 110.6 . .
C1 C2 H2B 110.6 . .
H2A C2 H2B 108.7 . .
C15 C14 C13 120.4(2) . .
C15 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
C4 C5 H5 120.0 . .
C6 C5 C4 120.0(2) . .
C6 C5 H5 120.0 . .
C19 C24 H24 120.1 . .
C19 C24 C23 119.8(3) . .
C23 C24 H24 120.1 . .
C21 C20 H20 120.5 . .
C21 C20 C19 118.9(3) . .
C19 C20 H20 120.5 . .
C21 C22 H22 120.2 . .
C21 C22 C23 119.6(3) . .
C23 C22 H22 120.2 . .
C24 C19 C20 120.7(3) . .
C24 C19 H19 119.6 . .
C20 C19 H19 119.6 . .
C24 C23 C22 120.0(3) . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
O1 Be2 Cl2 112.10(15) 2_667 .
O3 Be2 Cl2 112.98(16) . .
O3 Be2 O1 104.00(17) . 2_667
O4 Be2 Cl2 113.47(16) . .
O4 Be2 O1 106.40(17) . 2_667
O4 Be2 O3 107.21(17) . .
O4 Be3 Cl1 115.67(16) . .
O4 Be3 O7 113.67(18) . .
O4 Be3 O5 94.14(16) . .
O7 Be3 Cl1 114.03(17) . .
O7 Be3 O5 110.51(17) . .
O5 Be3 Cl1 106.66(14) . .
O1 Be1 O2 94.77(15) . .
O3 Be1 O1 117.23(18) . .
O3 Be1 O2 96.85(16) . .
O7 Be1 O1 116.01(19) . .
O7 Be1 O3 113.73(18) . .
O7 Be1 O2 114.94(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl2 Be2 2.001(3) .
Cl1 Be3 1.988(3) .
O1 C8 1.370(3) .
O1 Be2 1.650(3) 2_667
O1 Be1 1.629(3) .
O3 C1 1.442(3) .
O3 Be2 1.622(3) .
O3 Be1 1.593(3) .
O4 C18 1.435(3) .
O4 Be2 1.621(3) .
O4 Be3 1.598(3) .
O7 C9 1.441(3) .
O7 Be3 1.599(3) .
O7 Be1 1.574(3) .
O5 C16 1.400(3) .
O5 C17 1.462(3) .
O5 Be3 1.763(3) .
O6 C11 1.378(3) .
O6 C10 1.443(3) .
O2 C3 1.421(3) .
O2 C2 1.467(3) .
O2 Be1 1.803(3) .
C16 C11 1.388(3) .
C16 C15 1.383(3) .
C11 C12 1.388(3) .
C8 C3 1.390(3) .
C8 C7 1.382(3) .
C15 H15 0.9500 .
C15 C14 1.388(3) .
C3 C4 1.378(3) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C9 C10 1.509(3) .
C7 H7 0.9500 .
C7 C6 1.388(3) .
C12 H12 0.9500 .
C12 C13 1.387(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C17 C18 1.506(3) .
C4 H4 0.9500 .
C4 C5 1.402(3) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C6 H6 0.9500 .
C6 C5 1.387(4) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.502(3) .
C13 H13 0.9500 .
C13 C14 1.388(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C21 H21 0.9500 .
C21 C20 1.355(4) .
C21 C22 1.358(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C14 H14 0.9500 .
C5 H5 0.9500 .
C24 H24 0.9500 .
C24 C19 1.345(4) .
C24 C23 1.370(4) .
C20 H20 0.9500 .
C20 C19 1.413(4) .
C22 H22 0.9500 .
C22 C23 1.402(4) .
C19 H19 0.9500 .
C23 H23 0.9500 .
Be2 O1 1.650(3) 2_667
