A structural study of alkaline earth metal complexes with hybrid disila-crown ethers
Dankert, Fabian; Reuter, Kirsten; Donsbach, Carsten; von Hänisch, Carsten; Dalton Trans.  (2017) –; doi:10.1039/C6DT04018G

data_7041309
_publ_section_title
;
 A structural study of alkaline earth metal complexes with hybrid
 disila-crown ethers
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04018G
_journal_year                    2017
_chemical_formula_moiety         'C16 H32 Ba F6 O12 S2 Si2'
_chemical_formula_sum            'C16 H32 Ba F6 O12 S2 Si2'
_chemical_formula_weight         788.05
_chemical_properties_physical    ', Moisture-sensitive'
_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
_audit_creation_date             2016-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-03 deposited with the CCDC.
2016-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                72.5040(10)
_cell_angle_beta                 86.902(2)
_cell_angle_gamma                89.5490(10)
_cell_formula_units_Z            4
_cell_length_a                   9.7531(4)
_cell_length_b                   17.5485(8)
_cell_length_c                   18.5666(8)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.81
_cell_measurement_theta_min      2.41
_cell_volume                     3026.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103763
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.840
_diffrn_reflns_theta_min         2.259
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1426 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.5443.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.246
_refine_diff_density_max         1.030
_refine_diff_density_min         -2.699
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         18918
_refine_ls_number_restraints     824
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0237
_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/[\s^2^(Fo^2^)+(0.0176P)^2^+2.2114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17003
_reflns_number_total             18918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04018g2.cif
_cod_data_source_block           compound6
_cod_database_code               7041309
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-S5
 1.824 with sigma of 0.02
 C33-S5
 1.824 with sigma of 0.02
 C35-S7
 1.824 with sigma of 0.02
 C35-S7
 1.824 with sigma of 0.02
 C16-S2
 1.824 with sigma of 0.02
 C15-S1
 1.824 with sigma of 0.02
 C18-S4
 1.824 with sigma of 0.02
 C17-S3
 1.824 with sigma of 0.02
 C33-F13 \\sim C33-F15 \\sim C33-F14
 with sigma of 0.02
 F13-F15 \\sim F15-F14 \\sim F14-F13
 with sigma of 0.04
 S5-F13 \\sim S5-F15 \\sim S5-F14
 with sigma of 0.04
 S5-O27 \\sim S5-O26 \\sim S5-O25
 with sigma of 0.02
 O27-O26 \\sim O26-O25 \\sim O27-O25
 with sigma of 0.04
 C33-O27 \\sim C33-O26 \\sim C33-O25
 with sigma of 0.04
 C33-F13 \\sim C33-F15 \\sim C33-F14
 with sigma of 0.02
 F13-F15 \\sim F15-F14 \\sim F14-F13
 with sigma of 0.04
 S5-F13 \\sim S5-F15 \\sim S5-F14
 with sigma of 0.04
 S5-O27 \\sim S5-O26 \\sim S5-O25
 with sigma of 0.02
 O27-O26 \\sim O26-O25 \\sim O27-O25
 with sigma of 0.04
 C33-O27 \\sim C33-O26 \\sim C33-O25
 with sigma of 0.04
 C35-F20 \\sim C35-F21 \\sim C35-F19
 with sigma of 0.02
 F20-F21 \\sim F21-F19 \\sim F19-F20
 with sigma of 0.04
 S7-F20 \\sim S7-F21 \\sim S7-F19
 with sigma of 0.04
 S7-O33 \\sim S7-O32 \\sim S7-O31
 with sigma of 0.02
 O33-O32 \\sim O32-O31 \\sim O33-O31
 with sigma of 0.04
 C35-O33 \\sim C35-O32 \\sim C35-O31
 with sigma of 0.04
 C35-F20 \\sim C35-F21 \\sim C35-F19
 with sigma of 0.02
 F20-F21 \\sim F21-F19 \\sim F19-F20
 with sigma of 0.04
 S7-F20 \\sim S7-F21 \\sim S7-F19
 with sigma of 0.04
 S7-O33 \\sim S7-O32 \\sim S7-O31
 with sigma of 0.02
 O33-O32 \\sim O32-O31 \\sim O33-O31
 with sigma of 0.04
 C35-O33 \\sim C35-O32 \\sim C35-O31
 with sigma of 0.04
 C16-F6 \\sim C16-F4 \\sim C16-F5
 with sigma of 0.02
 F6-F4 \\sim F4-F5 \\sim F5-F6
 with sigma of 0.04
 S2-F6 \\sim S2-F4 \\sim S2-F5
 with sigma of 0.04
 S2-O10 \\sim S2-O11 \\sim S2-O12
 with sigma of 0.02
 O10-O11 \\sim O11-O12 \\sim O10-O12
 with sigma of 0.04
 C16-O10 \\sim C16-O11 \\sim C16-O12
 with sigma of 0.04
 C15-F2 \\sim C15-F1 \\sim C15-F3
 with sigma of 0.02
 F2-F1 \\sim F1-F3 \\sim F3-F2
 with sigma of 0.04
 S1-F2 \\sim S1-F1 \\sim S1-F3
 with sigma of 0.04
 S1-O9 \\sim S1-O8 \\sim S1-O7
 with sigma of 0.02
 O9-O8 \\sim O8-O7 \\sim O9-O7
 with sigma of 0.04
 C15-O9 \\sim C15-O8 \\sim C15-O7
 with sigma of 0.04
 C18-F12 \\sim C18-F10 \\sim C18-F11
 with sigma of 0.02
 F12-F10 \\sim F10-F11 \\sim F11-F12
 with sigma of 0.04
 S4-F12 \\sim S4-F10 \\sim S4-F11
 with sigma of 0.04
 S4-O16 \\sim S4-O17 \\sim S4-O18
 with sigma of 0.02
 O16-O17 \\sim O17-O18 \\sim O16-O18
 with sigma of 0.04
 C18-O16 \\sim C18-O17 \\sim C18-O18
 with sigma of 0.04
 C17-F8 \\sim C17-F7 \\sim C17-F9
 with sigma of 0.02
 F8-F7 \\sim F7-F9 \\sim F9-F8
 with sigma of 0.04
 S3-F8 \\sim S3-F7 \\sim S3-F9
 with sigma of 0.04
 S3-O15 \\sim S3-O14 \\sim S3-O13
 with sigma of 0.02
 O15-O14 \\sim O14-O13 \\sim O15-O13
 with sigma of 0.04
 C17-O15 \\sim C17-O14 \\sim C17-O13
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C33 \\sim F13 \\sim F15 \\sim F14 \\sim S5 \\sim O27 \\sim O26 \\sim O25:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C33 \\sim F13 \\sim F15 \\sim F14 \\sim S5 \\sim O27 \\sim O26 \\sim O25:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C35 \\sim F20 \\sim F21 \\sim F19 \\sim S7 \\sim O33 \\sim O32 \\sim O31:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C35 \\sim F20 \\sim F21 \\sim F19 \\sim S7 \\sim O33 \\sim O32 \\sim O31:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C16 \\sim F6 \\sim F4 \\sim F5 \\sim S2 \\sim O10 \\sim O11 \\sim O12: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C15 \\sim F2 \\sim F1 \\sim F3 \\sim S1 \\sim O9 \\sim O8 \\sim O7: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C18 \\sim F12 \\sim F10 \\sim F11 \\sim S4 \\sim O16 \\sim O17 \\sim O18:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C17 \\sim F8 \\sim F7 \\sim F9 \\sim S3 \\sim O15 \\sim O14 \\sim O13: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C15) = Uanis(C17)
Uanis(C36) = Uanis(C34)
Uanis(C33) = Uanis(C35)
4. Rigid body (RIGU) restrains
 C34, F17, F16, F18, S6, O29, O30, O28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33, F13, F15, F14, S5, O27, O26, O25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, F24, F23, F22, S8, O35, O36, O34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, F20, F21, F19, S7, O33, O32, O31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, F6, F4, F5, S2, O10, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, F2, F1, F3, S1, O9, O8, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18, F12, F10, F11, S4, O16, O17, O18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, F8, F7, F9, S3, O15, O14, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C36)=Sof(F24)=Sof(F23)=Sof(F22)=Sof(S8)=Sof(O35)=Sof(O36)=Sof(O34)=
 Sof(C35)=Sof(F20)=Sof(F21)=Sof(F19)=Sof(S7)=Sof(O33)=Sof(O32)=Sof(O31)=
 Sof(C18)=Sof(F12)=Sof(F10)=Sof(F11)=Sof(S4)=Sof(O16)=Sof(O17)=Sof(O18)=
 Sof(C17)=Sof(F8)=Sof(F7)=Sof(F9)=Sof(S3)=Sof(O15)=Sof(O14)=Sof(O13)=1-FVAR(1)
 Sof(C34)=Sof(F17)=Sof(F16)=Sof(F18)=Sof(S6)=Sof(O29)=Sof(O30)=Sof(O28)=
 Sof(C33)=Sof(F13)=Sof(F15)=Sof(F14)=Sof(S5)=Sof(O27)=Sof(O26)=Sof(O25)=
 Sof(C16)=Sof(F6)=Sof(F4)=Sof(F5)=Sof(S2)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C15)=
 Sof(F2)=Sof(F1)=Sof(F3)=Sof(S1)=Sof(O9)=Sof(O8)=Sof(O7)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H), C10(HA,H10B), C30(H30A,H30B), C23(H23A,H23B),
 C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C9(H9A,H9B), C27(H27A,H27B),
 C25(H25A,H25B), C12(H12A,H12B), C11(H11A,H11B), C26(H26A,H26B), C8(H8A,H8B),
 C5(H5A,H5B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C32(H32,H32B,H32C), C19(H19A,H19B,H19C),
  C14(H14A,H14B,H14C), C2(H2A,H2B,H2C), C20(H20A,H20B,H20C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              13918
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'