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_7041308
_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         'C20 H32 Ba F6 O12 S2 Si2'
_chemical_formula_sum            'C20 H32 Ba F6 O12 S2 Si2'
_chemical_formula_weight         836.09
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-29
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0173(4)
_cell_length_b                   10.3761(5)
_cell_length_c                   35.6495(16)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      30.445
_cell_measurement_theta_min      2.284
_cell_volume                     3335.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            32181
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.726
_diffrn_reflns_theta_min         2.271
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  0.9044
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1386 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.7381.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2946 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8616
_refine_ls_number_restraints     910
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+0.3489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0481
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7554
_reflns_number_total             8616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04018g2.cif
_cod_data_source_block           fd53_0m
_cod_database_code               7041308
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.023) H5B(0.023) H15A(0.029) H15B(0.029) H6A(0.022)
 H6B(0.022) H11(0.023) H8(0.023) H10(0.028) H9(0.028) H13A(0.022) H13B(0.022)
 H16A(0.036) H16B(0.036) H4A(0.028) H4B(0.028) H14A(0.024) H14B(0.024)
 H2A(0.057) H2B(0.057) H2C(0.057) H17A(0.067) H17B(0.067) H17C(0.067) H1A(0.06)
 H1B(0.06) H1C(0.06) H18A(0.066) H18B(0.066) H18C(0.066) H3A(0.031) H3B(0.031)
 Fixed X: H5A(0.3642) H5B(0.2024) H15A(0.8989) H15B(0.9684) H6A(0.1077)
 H6B(0.1757) H11(0.4175) H8(0.0521) H10(0.1805) H9(0.0005) H13A(0.6359)
 H13B(0.6033) H16A(0.849) H16B(0.9627) H4A(0.224) H4B(0.4015) H14A(0.8491)
 H14B(0.7833) H2A(0.3835) H2B(0.3559) H2C(0.4933) H17A(0.6196) H17B(0.6987)
 H17C(0.7945) H1A(0.6876) H1B(0.5446) H1C(0.6868) H18A(0.9121) H18B(0.9467)
 H18C(1.0007) H3A(0.3151) H3B(0.2255)
 Fixed Y: H5A(0.7472) H5B(0.7066) H15A(0.5962) H15B(0.5942) H6A(0.7324)
 H6B(0.8656) H11(0.9029) H8(0.8871) H10(0.9878) H9(0.9811) H13A(0.8886)
 H13B(0.7443) H16A(0.3949) H16B(0.3837) H4A(0.4909) H4B(0.5011) H14A(0.7648)
 H14B(0.8046) H2A(0.0744) H2B(0.0597) H2C(-0.0117) H17A(0.1546) H17B(0.0354)
 H17C(0.1336) H1A(0.1283) H1B(0.2035) H1C(0.2825) H18A(0.0924) H18B(0.2405)
 H18C(0.1786) H3A(0.2875) H3B(0.3424)
 Fixed Z: H5A(0.6936) H5B(0.7084) H15A(0.6149) H15B(0.5734) H6A(0.6464)
 H6B(0.6617) H11(0.5105) H8(0.6038) H10(0.4993) H9(0.5455) H13A(0.5382)
 H13B(0.5241) H16A(0.5619) H16B(0.5963) H4A(0.7211) H4B(0.7182) H14A(0.5474)
 H14B(0.5876) H2A(0.6347) H2B(0.6789) H2C(0.6595) H17A(0.5697) H17B(0.59)
 H17C(0.5653) H1A(0.7194) H1B(0.7344) H1C(0.7205) H18A(0.6577) H18B(0.6667)
 H18C(0.628) H3A(0.7055) H3B(0.6701)
;
_shelx_res_checksum              27808
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'