Synthesis of Structured Polysiloxazanes via Piers–Rubinsztajn Reaction
Ai, Liqing; Chen, Yi; He, Lijuan; Luo, Yongming; Li, Shuhong; Xu, Caihong; Chemical Communications  (2019) –; doi:10.1039/C9CC07312D

data_7124378
_publ_section_title
;
 Synthesis of Structured Polysiloxazanes via Piers--Rubinsztajn Reaction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07312D
_journal_year                    2019
_chemical_formula_moiety         'C60 H72 N2 O3 Si6'
_chemical_formula_sum            'C60 H72 N2 O3 Si6'
_chemical_formula_weight         1037.73
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.    2019-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                97.1130(10)
_cell_angle_beta                 100.5090(10)
_cell_angle_gamma                97.9270(10)
_cell_formula_units_Z            2
_cell_length_a                   9.76140(10)
_cell_length_b                   13.3279(2)
_cell_length_c                   22.9045(3)
_cell_measurement_reflns_used    27673
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.3410
_cell_measurement_theta_min      3.3720
_cell_volume                     2867.71(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.964
_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   -120.00 -49.00   0.50    0.10    --  -47.20 -48.00  82.00  142
  2  \w    -59.00  24.00   0.50    0.10    --  -47.20  48.00-129.00  166
  3  \w     56.00 120.00   0.50    0.10    --   47.20  48.00-129.00  128
  4  \w   -167.00 -86.00   0.50    0.20    --  -99.00 -48.00  82.00  162
  5  \w     31.00  77.00   0.50    0.20    --  103.25 -48.00  82.00   92
  6  \w     81.00 107.00   0.50    0.20    --  103.25 -48.00  82.00   52
  7  \w    140.00 167.00   0.50    0.20    --  103.25  48.00-129.00   54
  8  \w    100.00 135.00   0.50    0.20    --  103.25  48.00-129.00   70
  9  \w   -116.00 -81.00   0.50    0.10    --  -47.20-125.00  30.00   70
 10  \w   -116.00 -84.00   0.50    0.10    --  -47.20-125.00   0.00   64
 11  \w   -113.00 -87.00   0.50    0.10    --  -47.20-125.00  90.00   52
 12  \w    -24.00  46.00   0.50    0.10    --   47.20 -48.00  82.00  140
 13  \w     17.00  95.00   0.50    0.10    --   47.20-125.00 -30.00  156
 14  \w   -115.00 -89.00   0.50    0.20    --  -99.00  61.00  60.00   52
 15  \w   -118.00 -73.00   0.50    0.20    --  -99.00-125.00-120.00   90
 16  \w   -116.00 -51.00   0.50    0.20    --  -99.00 125.00 -30.00  130
 17  \w    -94.00 -69.00   0.50    0.20    --  -99.00  48.00-129.00   50
 18  \w   -162.00-121.00   0.50    0.20    --  -99.00-125.00-120.00   82
 19  \w     33.00 126.00   0.50    0.20    --  103.25 -77.00  90.00  186
 20  \w     78.00 104.00   0.50    0.20    --  103.25 -94.00-120.00   52
 21  \w    111.00 137.00   0.50    0.20    --  103.25  45.00 -60.00   52
 22  \w    142.00 168.00   0.50    0.20    --  103.25  45.00 -60.00   52
 23  \w     32.00 108.00   0.50    0.20    --  103.25 -94.00-150.00  152
 24  \w     32.00 117.00   0.50    0.20    --  103.25-125.00  90.00  170
 25  \w    107.00 169.00   0.50    0.20    --  103.25  15.00  30.00  124
 26  \w     34.00  92.00   0.50    0.20    --  103.25-125.00-150.00  116
 27  \w     63.00 104.00   0.50    0.20    --  103.25 -30.00-150.00   82
 28  \w     29.00 117.00   0.50    0.20    --  103.25 -15.00-120.00  176
 29  \w     33.00  59.00   0.50    0.20    --  103.25 -30.00-150.00   52
 30  \w     70.00 109.00   0.50    0.20    --  103.25 -94.00  90.00   78
 31  \w     74.00 116.00   0.50    0.20    --  103.25 -45.00-120.00   84
 32  \w     33.00  58.00   0.50    0.20    --  103.25 -94.00  90.00   50
 33  \w     35.00  63.00   0.50    0.20    --  103.25 -45.00-120.00   56
 34  \w     31.00 107.00   0.50    0.20    --  103.25 -94.00 -90.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051878000
_diffrn_orient_matrix_UB_12      -0.1050992000
_diffrn_orient_matrix_UB_13      -0.0376388000
_diffrn_orient_matrix_UB_21      -0.1424887000
_diffrn_orient_matrix_UB_22      -0.0388754000
_diffrn_orient_matrix_UB_23      0.0160576000
_diffrn_orient_matrix_UB_31      -0.0784312000
_diffrn_orient_matrix_UB_32      0.0372719000
_diffrn_orient_matrix_UB_33      -0.0558322000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34331
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.355
_diffrn_reflns_theta_min         3.388
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.223
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         11438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0492P)^2^+1.8438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10993
_reflns_number_total             11438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07312d2.cif
_cod_data_source_block           tx360
_cod_database_code               7124378
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNOSi
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Si6, C57
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Others
 Sof(H59C)=Sof(H59D)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(1)
 Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C55(H55A,H55B), C57(H57A,H57B),
 C59(H59A,H59B), C59(H59C,H59D)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C56(H56A,H56B,H56C),
 C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C60A(H60D,H60E,H60F)
;
_shelx_res_checksum              34152
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.835