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_1549875
_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         'C24 H22 Cl N O6'
_chemical_formula_sum            'C24 H22 Cl N O6'
_chemical_formula_weight         455.88
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-21
_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                90
_cell_angle_beta                 92.9404(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.33701(10)
_cell_length_b                   17.9259(3)
_cell_length_c                   21.5579(4)
_cell_measurement_reflns_used    11255
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.1660
_cell_measurement_theta_min      3.1420
_cell_volume                     2059.74(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 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -81.00  24.00   1.00    1.00    --  -41.80  96.00 164.00  105
  2  \w     -2.00  81.00   1.00    1.00    --   41.80 -96.00  56.00   83
  3  \w    101.00 178.00   1.00    1.00    --  109.13  96.00 164.00   77
  4  \w     27.00 110.00   1.00    1.00    --  109.13 -96.00  56.00   83
  5  \w   -114.00 -14.00   1.00    1.00    --  -41.80 -57.00  60.00  100
  6  \w    -50.00  32.00   1.00    1.00    --  -41.80  38.00 -60.00   82
  7  \w    -50.00  32.00   1.00    1.00    --  -41.80  38.00-150.00   82
  8  \w     33.00  91.00   1.00    1.00    --  109.13 -30.00 -90.00   58
  9  \w     33.00  91.00   1.00    1.00    --  109.13 -30.00-180.00   58
 10  \w     33.00  91.00   1.00    1.00    --  109.13 -30.00 120.00   58
 11  \w     36.00  98.00   1.00    1.00    --  109.13 -45.00  60.00   62
 12  \w     36.00 121.00   1.00    1.00    --  109.13-125.00-180.00   85
 13  \w     36.00  98.00   1.00    1.00    --  109.13 -45.00-120.00   62
 14  \w     36.00  98.00   1.00    1.00    --  109.13 -45.00  90.00   62
 15  \w     33.00  91.00   1.00    1.00    --  109.13 -30.00   0.00   58
 16  \w   -114.00 -14.00   1.00    1.00    --  -41.80 -57.00 -60.00  100
 17  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00 -90.00  109
 18  \w   -114.00 -14.00   1.00    1.00    --  -41.80 -57.00-180.00  100
 19  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00 150.00  109
 20  \w     77.00 178.00   1.00    1.00    --  109.13  77.00-120.00  101
 21  \w     81.00 178.00   1.00    1.00    --  109.13  30.00-120.00   97
 22  \w     56.00 178.00   1.00    1.00    --  109.13  15.00 150.00  122
 23  \w     83.00 178.00   1.00    1.00    --  109.13  45.00-180.00   95
 24  \w     56.00 178.00   1.00    1.00    --  109.13  15.00   0.00  122
 25  \w     80.00 178.00   1.00    1.00    --  109.13  61.00   0.00   98
 26  \w     26.00 109.00   1.00    1.00    --  109.13 -94.00-120.00   83
 27  \w     77.00 178.00   1.00    1.00    --  109.13  77.00  30.00  101
 28  \w    -96.00  -2.00   1.00    1.00    --  -41.80 125.00 -30.00   94
 29  \w   -116.00 -17.00   1.00    1.00    --  -41.80 -38.00 -90.00   99
 30  \w   -118.00  -9.00   1.00    1.00    --  -41.80 -77.00  30.00  109
 31  \w      9.00 118.00   1.00    1.00    --   41.80  77.00 -60.00  109
 32  \w     77.00 178.00   1.00    1.00    --  109.13  77.00 120.00  101
 33  \w     80.00 178.00   1.00    1.00    --  109.13  61.00 -30.00   98
 34  \w     26.00 109.00   1.00    1.00    --  109.13 -94.00 -30.00   83
 35  \w     77.00 178.00   1.00    1.00    --  109.13  77.00 -90.00  101
 36  \w     80.00 105.00   1.00    1.00    --  109.13  61.00-180.00   25
 37  \w     77.00 178.00   1.00    1.00    --  109.13  77.00  60.00  101
;
_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      0.1509264000
_diffrn_orient_matrix_UB_12      0.0279252000
_diffrn_orient_matrix_UB_13      0.0582892000
_diffrn_orient_matrix_UB_21      0.1369467000
_diffrn_orient_matrix_UB_22      -0.0755389000
_diffrn_orient_matrix_UB_23      0.0051874000
_diffrn_orient_matrix_UB_31      0.2047933000
_diffrn_orient_matrix_UB_32      0.0299961000
_diffrn_orient_matrix_UB_33      -0.0412316000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.465
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.980
_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    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.340
_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     291
_refine_ls_number_reflns         4238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0875P)^2^+0.8499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3338
_reflns_number_total             4238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01037d2.cif
_cod_data_source_block           rh062
_cod_depositor_comments
'Adding full bibliography for 1549874--1549876.cif.'
_cod_database_code               1549875
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C24 H22 Cl N O6'
_reflns_odcompleteness_completeness 99.95
_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), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              837
_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 1.617
_oxdiff_exptl_absorpt_empirical_full_min 0.685