Straightforward synthesis of novel cyclic metallasiloxanes supported by an N,C,N-chelating ligand.
Fridrichová, Adéla; Mairychová, Barbora; Padělková, Zdeňka; Lyčka, Antonín; Jurkschat, Klaus; Jambor, Roman; Dostál, Libor; Dalton transactions (Cambridge, England : 2003) 42 (2013) 16403–16411; doi:10.1039/c3dt52230j

data_7023989
_publ_section_title
;
 Straightforward synthesis of novel cyclic metallasiloxanes supported by
 an N,C,N-chelating ligand.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16403
_journal_page_last               16411
_journal_paper_doi               10.1039/c3dt52230j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C60 H68 N4 O4 Si2 Sn2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C60.5 H69 Cl N4 O4 Si2 Sn2'
_chemical_formula_weight         1245.21
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.403(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5356(3)
_cell_length_b                   16.2802(3)
_cell_length_c                   21.3586(4)
_cell_measurement_reflns_used    18612
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      2.08
_cell_volume                     5997.29(19)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.32.37''
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd.,Version 1.171.32.37''
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.32.37''
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'XcaliburS CCD Diffractometer'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29851
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         11137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                8759
_reflns_number_total             11137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52230j.txt
_cod_data_source_block           compound5*0.5CH2Cl2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C60.50 H69 Cl N4 O4 Si2 Sn2'
_cod_database_code               7023989