Selective Derivatization and Characterization of Bifunctional “Janus-Type” Cyclotetrasiloxanes
Panisch, Robin; Bassindale, Alan R.; Korlyukov, Alexander A.; Pitak, Mateusz B.; Coles, Simon J.; Taylor, Peter G.; Organometallics 32 (2013) 1732–; doi:10.1021/om301158w

data_4080386
_publ_section_title
;
 Selective Derivatization and Characterization of Bifunctional
 &#x201C;Janus-Type&#x201D; Cyclotetrasiloxanes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1732
_journal_paper_doi               10.1021/om301158w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C40 H52 I4 O8 Si8'
_chemical_formula_sum            'C40 H52 I4 O8 Si8'
_chemical_formula_weight         1393.14
_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                 96.973(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2691(15)
_cell_length_b                   21.9669(8)
_cell_length_c                   11.5215(4)
_cell_measurement_reflns_used    22662
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     5594.4(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22316
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.442
_exptl_absorpt_correction_T_max  0.3748
_exptl_absorpt_correction_T_min  0.2454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         9678
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+104.7269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                8507
_reflns_number_total             9678
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om301158w_si_001.cif
_cod_data_source_block           derivative16r2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4080386