The coordination behaviour and reactivity of partially silicon based crown ethers towards beryllium chloride.
Buchner, Magnus R.; Müller, Matthias; Dankert, Fabian; Reuter, Kirsten; von Hänisch, Carsten; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16393–16397; doi:10.1039/c8dt03963a

data_7047764
_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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.0414P)^2^+1.6165P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              3639
_olex2_submission_special_instructions 'No special instructions were received'