Aluminum-Based Initiators from Thiols for Epoxide Polymerizations
Safaie, Niloofar; Rawal, Bandana; Ohno, Kohji; Ferrier, Robert C.; Macromolecules 53 (2020) 8181–8191; doi:10.1021/acs.macromol.0c00464

data_1559235
_publ_section_title
;
 Aluminum-Based Initiators from Thiols for Epoxide Polymerizations
;
_journal_issue                   19
_journal_name_full               Macromolecules
_journal_page_first              8181
_journal_page_last               8191
_journal_paper_doi               10.1021/acs.macromol.0c00464
_journal_volume                  53
_journal_year                    2020
_chemical_formula_moiety         'C9 H12 Al Cl S'
_chemical_formula_sum            'C9 H12 Al Cl S'
_chemical_formula_weight         214.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-25
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8139(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.40835(19)
_cell_length_b                   13.7459(3)
_cell_length_c                   7.12221(12)
_cell_measurement_reflns_used    7475
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.7560
_cell_measurement_theta_min      3.1800
_cell_volume                     1103.70(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXT (Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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    127.00 178.00   0.50    0.15    --  107.11  57.00 -30.00  102
  2  \w    114.00 177.00   0.50    0.15    --  107.11  37.00 -90.00  126
  3  \w    131.00 174.00   0.50    0.15    --  107.11  77.00-150.00   86
  4  \w    129.00 175.00   0.50    0.15    --  107.11  57.00-180.00   92
  5  \w    130.00 161.00   0.50    0.15    --  107.11  19.00-180.00   62
  6  \w    -61.00  15.00   0.50    0.05    --  -47.45  57.00  30.00  152
  7  \w    -26.00  28.00   0.50    0.05    --  -47.45  19.00  90.00  108
  8  \w    -10.00  21.00   0.50    0.05    --  -47.45  19.00   0.00   62
  9  \w    -19.00  23.00   0.50    0.05    --  -47.45  19.00 -30.00   84
 10  \w    -25.00  26.00   0.50    0.05    --  -47.45  19.00 -90.00  102
 11  \w     32.00  60.00   0.50    0.05    --   47.45-111.00 -11.00   56
 12  \w     38.00  64.00   0.50    0.15    --  107.11 -99.00  30.00   52
 13  \w     52.00  78.00   0.50    0.15    --  107.11-111.00 -11.00   52
 14  \w     63.00 103.00   0.50    0.15    --  107.11 -99.00   0.00   80
 15  \w     71.00 105.00   0.50    0.15    --  107.11 -99.00  90.00   68
 16  \w     47.00  92.00   0.50    0.15    --  107.11 -99.00 150.00   90
 17  \w     70.00 102.00   0.50    0.15    --  107.11 -99.00  30.00   64
 18  \w     36.00  62.00   0.50    0.15    --  107.11 -99.00  90.00   52
 19  \w     41.00  75.00   0.50    0.15    --  107.11 -99.00-120.00   68
 20  \w     81.00 106.00   0.50    0.15    --  107.11 -99.00-120.00   50
 21  \w     81.00 106.00   0.50    0.15    --  107.11 -99.00-180.00   50
 22  \w     72.00 104.00   0.50    0.15    --  107.11 -77.00-150.00   64
 23  \w     37.00  62.00   0.50    0.15    --  107.11 -77.00-150.00   50
 24  \w     38.00  63.00   0.50    0.15    --  107.11 -57.00 -90.00   50
 25  \w     35.00  63.00   0.50    0.15    --  107.11 -57.00-120.00   56
 26  \w     38.00  63.00   0.50    0.15    --  107.11 -57.00   0.00   50
 27  \w     36.00  62.00   0.50    0.15    --  107.11 -57.00 -60.00   52
 28  \w     70.00  95.00   0.50    0.15    --  107.11 -77.00  30.00   50
 29  \w    -26.00  16.00   0.50    0.05    --   47.45 -19.00  90.00   84
 30  \w     38.00  96.00   0.50    0.15    --  107.11 -77.00 150.00  116
 31  \w     35.00  61.00   0.50    0.15    --  107.11 -57.00 150.00   52
 32  \w     35.00  61.00   0.50    0.15    --  107.11 -57.00  90.00   52
 33  \w    120.00 146.00   0.50    0.15    --  107.11 125.00  60.00   52
 34  \w    153.00 178.00   0.50    0.15    --  107.11 125.00  60.00   50
 35  \w    112.00 151.00   0.50    0.15    --  107.11 111.00  82.00   78
 36  \w    -45.00  -2.00   0.50    0.05    --  -47.45 111.00  82.00   86
 37  \w    -82.00 -43.00   0.50    0.15    --  -86.25 111.00  82.00   78
 38  \w    -43.00 -18.00   0.50    0.15    --  -86.25  37.00  30.00   50
 39  \w    -42.00 -17.00   0.50    0.15    --  -86.25  37.00-120.00   50
 40  \w   -157.00-130.00   0.50    0.15    --  -86.25 -77.00-150.00   54
 41  \w   -159.00-134.00   0.50    0.15    --  -86.25 -77.00-180.00   50
 42  \w   -152.00-122.00   0.50    0.15    --  -86.25 -37.00-150.00   60
 43  \w   -159.00-134.00   0.50    0.15    --  -86.25 -57.00 -90.00   50
 44  \w   -157.00-127.00   0.50    0.15    --  -86.25 -57.00 -60.00   60
 45  \w   -159.00-134.00   0.50    0.15    --  -86.25 -37.00 120.00   50
 46  \w   -151.00-115.00   0.50    0.15    --  -86.25 -37.00  90.00   72
 47  \w   -133.00-108.00   0.50    0.15    --  -86.25-111.00 -11.00   50
 48  \w   -159.00-134.00   0.50    0.15    --  -86.25 -99.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0817517000
_diffrn_orient_matrix_UB_12      -0.0896290000
_diffrn_orient_matrix_UB_13      -0.0089886000
_diffrn_orient_matrix_UB_21      0.1062793000
_diffrn_orient_matrix_UB_22      -0.0632949000
_diffrn_orient_matrix_UB_23      0.0857530000
_diffrn_orient_matrix_UB_31      -0.0261828000
_diffrn_orient_matrix_UB_32      0.0229905000
_diffrn_orient_matrix_UB_33      0.2011799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1069
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            12098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.926
_diffrn_reflns_theta_min         3.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.163
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0950P)^2^+0.5505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2101
_reflns_number_total             2289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c00464_si_001.cif
_cod_data_source_block           rf220a
_cod_depositor_comments
'Adding full bibliography for 1559235--1559237.cif.'
_cod_original_cell_volume        1103.70(3)
_cod_database_code               1559235
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C9 H12 Al1 Cl1 S1'
_chemical_oxdiff_usercomment     ClBnSAlMe2
_shelx_estimated_absorpt_t_max   0.413
_shelx_estimated_absorpt_t_min   0.218
_reflns_odcompleteness_completeness 100.00
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              85143
_shelx_hkl_checksum              82567
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'solvent frozen at liquid nitrogen on nylon loop'
_olex2_submission_original_sample_id ClBnSAlMe2
_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 7.941
_oxdiff_exptl_absorpt_empirical_full_min 0.338