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_7041307
_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         'C12 H28 Br2 Mg O5 Si2'
_chemical_formula_sum            'C12 H28 Br2 Mg O5 Si2'
_chemical_formula_weight         492.65
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-27
_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            8
_cell_length_a                   10.8339(6)
_cell_length_b                   14.1089(7)
_cell_length_c                   27.7507(14)
_cell_measurement_reflns_used    6117
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.191
_cell_measurement_theta_min      2.385
_cell_volume                     4241.8(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22357
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.271
_diffrn_reflns_theta_min         2.385
_exptl_absorpt_coefficient_mu    3.980
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.8351.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0322
_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/[\s^2^(Fo^2^)+(0.0116P)^2^+5.0851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3003
_reflns_number_total             3841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04018g2.cif
_cod_data_source_block           compound3
_cod_database_code               7041307
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.019) H5B(0.019) H8A(0.023) H8B(0.023) H9A(0.018) H9B(0.018)
 H10A(0.024) H10B(0.024) H10C(0.024) H13A(0.017) H13B(0.017) H14A(0.028)
 H14B(0.028) H14C(0.028) H15A(0.019) H15B(0.019) H17A(0.024) H17B(0.024)
 H19A(0.016) H19B(0.016) H21A(0.038) H21B(0.038) H21C(0.038) H22A(0.018)
 H22B(0.018) H23A(0.041) H23B(0.041) H23C(0.041)
 Fixed X: H5A(0.2841) H5B(0.2968) H8A(-0.2167) H8B(-0.3219) H9A(-0.269) H9B(-
 0.2267) H10A(0.1661) H10B(0.2903) H10C(0.2975) H13A(-0.1768) H13B(-0.0632)
 H14A(0.454) H14B(0.4571) H14C(0.4068) H15A(-0.0874) H15B(-0.0638) H17A(-
 0.3309) H17B(-0.3524) H19A(0.021) H19B(-0.0753) H21A(0.2373) H21B(0.1482)
 H21C(0.2777) H22A(0.1045) H22B(0.1799) H23A(0.1419) H23B(0.0219) H23C(0.0219)
 Fixed Y: H5A(0.5574) H5B(0.4606) H8A(0.6807) H8B(0.6709) H9A(0.4253)
 H9B(0.3658) H10A(0.2483) H10B(0.2922) H10C(0.2106) H13A(0.7279) H13B(0.7331)
 H14A(0.346) H14B(0.4115) H14C(0.4534) H15A(0.3333) H15B(0.4445) H17A(0.5051)
 H17B(0.5569) H19A(0.6958) H19B(0.61) H21A(0.4132) H21B(0.3395) H21C(0.3046)
 H22A(0.4834) H22B(0.5809) H23A(0.1515) H23B(0.1857) H23C(0.1856)
 Fixed Z: H5A(0.1848) H5B(0.2148) H8A(0.1083) H8B(0.149) H9A(0.0435)
 H9B(0.0902) H10A(0.1934) H10B(0.2153) H10C(0.1753) H13A(0.2093) H13B(0.1719)
 H14A(0.105) H14B(0.1521) H14C(0.1022) H15A(0.0277) H15B(0.0196) H17A(0.1363)
 H17B(0.0853) H19A(0.2479) H19B(0.2545) H21A(0.0137) H21B(-0.013) H21C(0.0083)
 H22A(0.2503) H22B(0.2568) H23A(0.0716) H23B(0.0428) H23C(0.1005)
;
_shelx_res_checksum              49411
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'