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_7230175
_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         'C17 H34 N2 O6 Si4'
_chemical_formula_sum            'C17 H34 N2 O6 Si4'
_chemical_formula_weight         474.82
_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             2017-12-14
_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                86.843(5)
_cell_angle_beta                 87.831(6)
_cell_angle_gamma                84.815(6)
_cell_formula_units_Z            2
_cell_length_a                   6.8337(6)
_cell_length_b                   8.3901(5)
_cell_length_c                   22.7542(15)
_cell_measurement_reflns_used    2290
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      26.1790
_cell_measurement_theta_min      1.7790
_cell_volume                     1296.60(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -24.00  23.00   1.00   15.00    --  -15.76 -99.00  60.00   47
  2  \w     24.00  54.00   1.00   15.00    --   17.94 -99.00 -60.00   30
  3  \w    -30.00  51.00   1.00   15.00    --  -15.76  77.00   0.00   81
  4  \w     56.00  83.00   1.00   15.00    --   17.94 178.00-180.00   27
  5  \w    -86.00  13.00   1.00   15.00    --  -15.76 -19.00-150.00   99
  6  \w    -83.00  -2.00   1.00   15.00    --  -15.76 -57.00 150.00   81
;
_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      0.0008273000
_diffrn_orient_matrix_UB_12      0.0112489000
_diffrn_orient_matrix_UB_13      -0.0311298000
_diffrn_orient_matrix_UB_21      0.1032177000
_diffrn_orient_matrix_UB_22      0.0043848000
_diffrn_orient_matrix_UB_23      -0.0004284000
_diffrn_orient_matrix_UB_31      0.0148113000
_diffrn_orient_matrix_UB_32      -0.0841400000
_diffrn_orient_matrix_UB_33      -0.0025461000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9890
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0749
_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^)+(0.0449P)^2^+0.1982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                3542
_reflns_number_total             5307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ra00707a2.cif
_cod_data_source_block           shi_3282_elpe
_cod_database_code               7230175
_chemical_oxdiff_formula         'C20 H20 O6 N2 Si4'
_chemical_oxdiff_usercomment     D4NO2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C)
;
_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 1.141
_oxdiff_exptl_absorpt_empirical_full_min 0.882