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_7041305
_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 Ca F6 O12 S2 Si2'
_chemical_formula_sum            'C16 H32 Ca F6 O12 S2 Si2'
_chemical_formula_weight         690.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
;
2016-11-22 deposited with the CCDC.
2016-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.04(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9460(18)
_cell_length_b                   34.272(7)
_cell_length_c                   9.6976(19)
_cell_measurement_reflns_used    13818
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.235
_cell_volume                     2896.6(11)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2-T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13664
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.806
_diffrn_reflns_theta_max         24.806
_diffrn_reflns_theta_min         2.236
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.8737
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-Area'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       plank
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0693P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             4991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04018g2.cif
_cod_data_source_block           compound4
_cod_database_code               7041305
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C11(H11A,H11B), C4(H4A,H4B), C12(H12A,H12B), C7(H7A,H7B), C8(H8A,
 H8B), C5(H5A,H5B), C6(H6A,H6B), C10(H10A,H10B), C9(H9A,H9B)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              87836
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'