“Carbolong” polymers with near infrared triggered, spatially resolved and rapid self-healing properties
Zhang, Huan; Zhao, Haibo; Zhuo, Kaiyue; Hua, Yuhui; Chen, Jiangxi; He, Xumin; Weng, Wengui; Xia, Haiping; Polymer Chemistry 10 (2019) 386–; doi:10.1039/C8PY01482E

data_1550360
_publ_section_title
;
 &#x201C;Carbolong&#x201D; polymers with near infrared triggered,
 spatially resolved and rapid self-healing properties
;
_journal_issue                   3
_journal_name_full               'Polymer Chemistry'
_journal_page_first              386
_journal_paper_doi               10.1039/C8PY01482E
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C74 H70 O2 Os P3, 3(C H2 Cl2), B F4'
_chemical_formula_sum            'C77 H76 B Cl6 F4 O2 Os P3'
_chemical_formula_weight         1615.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-19 deposited with the CCDC.
2018-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.19810(10)
_cell_length_b                   26.75170(10)
_cell_length_c                   21.82430(10)
_cell_measurement_reflns_used    42055
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.1570
_cell_measurement_theta_min      3.8710
_cell_volume                     7051.95(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -85.00 -60.00   0.50    0.50    --  -46.87 141.00-118.00   50
  2  \w   -118.00 -93.00   0.50    0.50    --  -46.87-129.00  -3.00   50
  3  \w    -90.00 -65.00   0.50    0.50    --  -46.87-141.00-176.00   50
  4  \w    -94.00 -42.00   0.50    0.50    --  -46.87 129.00  69.00  104
  5  \w     48.00  73.00   0.50    0.50    --   46.87-141.00-176.00   50
  6  \w     42.00  67.00   0.50    0.50    --   46.87-129.00  -3.00   50
  7  \w    -85.00 -60.00   0.50    1.50    --  -88.50 141.00-118.00   50
  8  \w    -79.00 -54.00   0.50    1.50    --  -88.50 129.00  69.00   50
  9  \w     53.00 120.00   0.50    1.50    --  110.00-129.00  -3.00  134
 10  \w    105.00 130.00   0.50    1.50    --  110.00 141.00-118.00   50
 11  \w     95.00 138.00   0.50    1.50    --  110.00 129.00  69.00   86
 12  \w     40.00 129.00   0.50    1.50    --  110.00-141.00-176.00  178
 13  \w    -62.00  21.00   0.50    0.50    --  -46.87  37.00 -30.00  166
 14  \w   -120.00 -72.00   0.50    0.50    --  -46.87-125.00  30.00   96
 15  \w   -119.00 -31.00   0.50    0.50    --  -46.87 -57.00   0.00  176
 16  \w   -101.00 -16.00   0.50    1.50    --  -88.50  45.00 120.00  170
 17  \w     55.00  81.00   0.50    1.50    --  110.00 -94.00-180.00   52
 18  \w     96.00 173.00   0.50    1.50    --  110.00  30.00   0.00  154
 19  \w    130.00 155.00   0.50    1.50    --  110.00  61.00 150.00   50
 20  \w     99.00 178.00   0.50    1.50    --  110.00  30.00  90.00  158
 21  \w     58.00 107.00   0.50    1.50    --  110.00 -94.00-150.00   98
 22  \w     43.00 125.00   0.50    1.50    --  110.00 -77.00-180.00  164
 23  \w     53.00  94.00   0.50    1.50    --  110.00 -61.00 -30.00   82
 24  \w     94.00 121.00   0.50    1.50    --  110.00  61.00 150.00   54
 25  \w     45.00 109.00   0.50    1.50    --  110.00 -30.00 -60.00  128
;
_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      -0.0060574000
_diffrn_orient_matrix_UB_12      -0.0483420000
_diffrn_orient_matrix_UB_13      -0.0387159000
_diffrn_orient_matrix_UB_21      -0.0010811000
_diffrn_orient_matrix_UB_22      -0.0311871000
_diffrn_orient_matrix_UB_23      0.0592394000
_diffrn_orient_matrix_UB_31      -0.1273927000
_diffrn_orient_matrix_UB_32      0.0025212000
_diffrn_orient_matrix_UB_33      -0.0085950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51957
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         3.887
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       needle
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.151
_refine_diff_density_min         -2.029
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         11985
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+33.4895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11660
_reflns_number_total             11985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py01482e3.cif
_cod_data_source_block           zhb-180809
_cod_depositor_comments          'Adding full bibliography for 1550360.cif.'
_cod_database_code               1550360
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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 O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C14(H14A,H14B), C13(H13A,H13B), C19(H19A,
 H19B), C16(H16A,H16B), C20(H20A,H20B), C15(H15A,H15B), C02J(H02C,H02G),
 C02L(H02H,H02I), C02M(H02J,H02K)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C00J(H00J), C00L(H00L), C10(H10), C6(H6), C00T(H00T), C00U(H00U),
 C00V(H00V), C00X(H00X), C00Z(H00Z), C012(H012), C013(H013), C014(H014),
 C016(H016), C017(H017), C018(H018), C01A(H01A), C01B(H01B), C5(H5), C01D(H01D),
  C01E(H01E), C3(H3), C01H(H01H), C01I(H01I), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01S(H01S),
 C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Z(H01Z), C8(H8),
  C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C028(H028),
 C029(H029), C02A(H02A), C02B(H02B), C02D(H02D), C02E(H02E), C02F(H02F)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2)
;
_shelx_res_checksum              56122
_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 3.101
_oxdiff_exptl_absorpt_empirical_full_min 0.433