Poly(2-oxazoline)s with pendant cubane groups
Glassner, Mathias; Verbraeken, Bart; Jerca, Valentin Victor; Van Hecke, Kristof; Tsanaktsidis, John; Hoogenboom, Richard; Polymer Chemistry 9 (2018) 4840–; doi:10.1039/C8PY01037D

data_1549874
_publ_section_title
;
 Poly(2-oxazoline)s with pendant cubane groups
;
_journal_issue                   39
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4840
_journal_paper_doi               10.1039/C8PY01037D
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C13 H13 N O3'
_chemical_formula_sum            'C13 H13 N O3'
_chemical_formula_weight         231.24
_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
_audit_creation_date             2015-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-07-09 deposited with the CCDC.
2018-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                71.126(6)
_cell_angle_beta                 76.243(6)
_cell_angle_gamma                77.203(6)
_cell_formula_units_Z            2
_cell_length_a                   5.8314(4)
_cell_length_b                   9.9500(6)
_cell_length_c                   10.2599(6)
_cell_measurement_reflns_used    2855
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.8420
_cell_measurement_theta_min      4.5880
_cell_volume                     540.33(6)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -91.00   7.00   1.00    1.00    --  -41.68 114.00-120.00   98
  2  \w     14.00  91.00   1.00    1.00    --   41.68-114.00 148.00   77
  3  \w     33.00 117.00   1.00    1.00    --  109.13-114.00 148.00   84
  4  \w    100.00 178.00   1.00    1.00    --  109.13 114.00-120.00   78
  5  \w    -50.00  33.00   1.00    1.00    --  -41.68  38.00-120.00   83
  6  \w    -50.00  33.00   1.00    1.00    --  -41.68  38.00 120.00   83
  7  \w   -122.00  -1.00   1.00    1.00    --  -41.68 -19.00 -60.00  121
  8  \w     23.00  98.00   1.00    1.00    --   41.68-125.00   0.00   75
  9  \w     36.00 121.00   1.00    1.00    --  109.13-125.00  30.00   85
 10  \w     26.00 109.00   1.00    1.00    --  109.13 -94.00  60.00   83
 11  \w     33.00  91.00   1.00    1.00    --  109.13 -30.00-180.00   58
 12  \w     80.00 178.00   1.00    1.00    --  109.13  61.00 -60.00   98
 13  \w     33.00  91.00   1.00    1.00    --  109.13 -30.00   0.00   58
 14  \w     36.00  98.00   1.00    1.00    --  109.13 -45.00 120.00   62
 15  \w     94.00 178.00   1.00    1.00    --  109.13 125.00   0.00   84
 16  \w     26.00 109.00   1.00    1.00    --  109.13 -94.00-120.00   83
 17  \w     36.00  98.00   1.00    1.00    --  109.13 -45.00 -30.00   62
 18  \w     36.00  98.00   1.00    1.00    --  109.13 -45.00-120.00   62
 19  \w     26.00 109.00   1.00    1.00    --  109.13 -94.00-180.00   83
 20  \w     81.00 178.00   1.00    1.00    --  109.13  30.00 120.00   97
 21  \w     81.00 178.00   1.00    1.00    --  109.13  30.00-180.00   97
 22  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 150.00  101
 23  \w   -118.00  -9.00   1.00    1.00    --  -41.68 -77.00   0.00  109
 24  \w   -118.00  -9.00   1.00    1.00    --  -41.68 -77.00 -90.00  109
 25  \w   -118.00  -9.00   1.00    1.00    --  -41.68 -77.00 120.00  109
 26  \w    -50.00  33.00   1.00    1.00    --  -41.68  38.00  30.00   83
 27  \w     14.00 115.00   1.00    1.00    --   41.68  57.00  90.00  101
 28  \w     81.00 178.00   1.00    1.00    --  109.13  30.00  30.00   97
 29  \w     80.00 178.00   1.00    1.00    --  109.13  61.00 120.00   98
 30  \w     80.00 178.00   1.00    1.00    --  109.13  61.00 -90.00   98
 31  \w     80.00 178.00   1.00    1.00    --  109.13  61.00 -30.00   98
 32  \w     80.00 178.00   1.00    1.00    --  109.13  61.00-150.00   98
 33  \w     83.00 178.00   1.00    1.00    --  109.13  45.00  60.00   95
 34  \w     83.00 178.00   1.00    1.00    --  109.13  45.00  30.00   95
 35  \w     80.00 178.00   1.00    1.00    --  109.13  61.00-120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1250753000
_diffrn_orient_matrix_UB_12      -0.0294669000
_diffrn_orient_matrix_UB_13      0.1543896000
_diffrn_orient_matrix_UB_21      0.1708443000
_diffrn_orient_matrix_UB_22      -0.1434049000
_diffrn_orient_matrix_UB_23      0.0369440000
_diffrn_orient_matrix_UB_31      0.1759689000
_diffrn_orient_matrix_UB_32      0.0775148000
_diffrn_orient_matrix_UB_33      0.0283894000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10257
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.228
_diffrn_reflns_theta_min         4.630
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1256P)^2^+0.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.2046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1580
_reflns_number_total             2195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01037d2.cif
_cod_data_source_block           rh061
_cod_depositor_comments
'Adding full bibliography for 1549874--1549876.cif.'
_cod_database_code               1549874
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C13 H13 N O3'
_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 Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              43957
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.222
_oxdiff_exptl_absorpt_empirical_full_min 0.613