Synthesis of novel cyclosiloxane monomers containing push–pull moieties and their anionic ring opening polymerization
Perju, Elena; Cuervo-Reyes, Eduardo; Shova, Sergiu; Opris, Dorina M.; RSC Advances 8 (2018) 7569–; doi:10.1039/C8RA00707A

data_7230176
_publ_section_title
;
 Synthesis of novel cyclosiloxane monomers containing push--pull moieties
 and their anionic ring opening polymerization
;
_journal_issue                   14
_journal_name_full               'RSC Advances'
_journal_page_first              7569
_journal_paper_doi               10.1039/C8RA00707A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C27 H44 N4 O8 Si4'
_chemical_formula_sum            'C27 H44 N4 O8 Si4'
_chemical_formula_weight         665.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-14 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                94.797(6)
_cell_angle_beta                 90.275(7)
_cell_angle_gamma                98.677(8)
_cell_formula_units_Z            2
_cell_length_a                   7.1467(8)
_cell_length_b                   8.3552(7)
_cell_length_c                   30.714(2)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.2610
_cell_measurement_theta_min      2.0000
_cell_volume                     1806.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     80.00 107.00   1.00   50.00    --   30.71 178.00 -90.00   27
  2  \w    -43.00  51.00   1.00   50.00    --   30.71 -38.00  30.00   94
  3  \w      0.00  95.00   1.00   50.00    --   30.71  38.00-150.00   95
  4  \w     87.00 113.00   1.00   50.00    --   30.71-178.00-150.00   26
  5  \w     48.00 101.00   1.00   50.00    --   30.71  57.00 -60.00   53
  6  \w     -5.00  73.00   1.00   50.00    --   30.71-105.00 -94.00   78
  7  \w    -22.00  73.00   1.00   50.00    --   30.71 -99.00   0.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0603738000
_diffrn_orient_matrix_UB_12      0.0480015000
_diffrn_orient_matrix_UB_13      0.0160642000
_diffrn_orient_matrix_UB_21      0.0722356000
_diffrn_orient_matrix_UB_22      0.0121762000
_diffrn_orient_matrix_UB_23      -0.0156664000
_diffrn_orient_matrix_UB_31      -0.0349264000
_diffrn_orient_matrix_UB_32      0.0705439000
_diffrn_orient_matrix_UB_33      -0.0058106000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            11991
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0947
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+1.8453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2282
_reflns_number_gt                3848
_reflns_number_total             5933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ra00707a2.cif
_cod_data_source_block           shi_3741_elpe
_cod_original_cell_volume        1806.3(3)
_cod_database_code               7230176
_chemical_oxdiff_formula         C30H30N4O6Si4
_chemical_oxdiff_usercomment     D4DRINO2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H13B-H21X
 2 with sigma of 0.1
 N4-C25X \\sim N4-C25
 with sigma of 0.01
 N2-C22X \\sim N2X-C22
 with sigma of 0.01
 N2-C19 \\sim N2X-C19X
 with sigma of 0.01
 Si2-O2X \\sim Si2-O2 \\sim Si3-O2X \\sim Si3-O2 \\sim Si3-O3X \\sim Si3-O3
\\sim Si4-O3X \\sim Si4-O3
 with sigma of 0.01
 Si3-C4 \\sim Si3-C4X \\sim Si3-C5 \\sim Si3-C5X
 with sigma of 0.01
 C16-C17 \\sim C17X-C16 \\sim C18-C17 \\sim C17X-C18X \\sim C18-C19 \\sim
C18X-C19X \\sim C19-C20 ~
 C20X-C19X \\sim C20-C21 \\sim C20X-C21X \\sim C21X-C16 \\sim C21-C16
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Si3 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C25X) = Uanis(C25) = Uanis(C26) = Uanis(C26X) = Uanis(C27) = Uanis(C27X)
= Uanis(C22) = Uanis(C22X) = Uanis(C23X) = Uanis(C23) = Uanis(C24X) =
Uanis(C24) = Uanis(N3) = Uanis(N2) = Uanis(N3X) = Uanis(N2X)
Uanis(O3) = Uanis(O3X) = Uanis(O2X) = Uanis(O2)
Uanis(C5X) = Uanis(C5) = Uanis(C4X) = Uanis(C4)
Uanis(C19) = Uanis(C19X) = Uanis(C18X) = Uanis(C18) = Uanis(C17X) = Uanis(C17)
= Uanis(C21X) = Uanis(C21) = Uanis(C20X) = Uanis(C20)
4. Others
 Sof(N2X)=Sof(N3X)=Sof(C17X)=Sof(H17X)=Sof(C18X)=Sof(H18X)=Sof(C19X)=Sof(C20X)=
 Sof(H20X)=Sof(C21X)=Sof(H21X)=Sof(C22X)=Sof(C23X)=Sof(H23X)=Sof(C24X)=
 Sof(H24X)=Sof(C25X)=Sof(C26X)=Sof(H26X)=Sof(C27X)=Sof(H27X)=1-FVAR(1)
 Sof(N2)=Sof(N3)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(C20)=
 Sof(H20)=Sof(C21)=Sof(H21)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C22)=FVAR(1)
 Sof(O2X)=Sof(O3X)=Sof(C4X)=Sof(H4XA)=Sof(H4XB)=Sof(H4XC)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=Sof(H5C)=1-FVAR(2)
 Sof(O2)=Sof(O3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5X)=Sof(H5XA)=
 Sof(H5XB)=Sof(H5XC)=FVAR(2)
5.a Riding coordinates:
 C13(H13A,H13B), C21X(H21X)
5.b Ternary CH refined with riding coordinates:
 C9(H9)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B), C14(H14A,H14B)
5.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26),
 C27(H27), C17X(H17X), C18X(H18X), C20X(H20X), C23X(H23X), C24X(H24X),
 C26X(H26X), C27X(H27X)
5.e Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C27,C22), C22X(C23X,C24X,C25X,C26X,C27X)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C4(H4A,H4B,H4C), C5X(H5XA,
 H5XB,H5XC), C4X(H4XA,H4XB,H4XC), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.722
_oxdiff_exptl_absorpt_empirical_full_min 0.600