Synthesis and properties investigation of hydroxyl functionalized polyisoprene prepared by cobalt catalyzed co-polymerization of isoprene and hydroxylmyrcene
Xu, Yuechao; Zhao, Junyi; Gan, Qiao; Ying, Weilun; Hu, Zhonghan; Tang, Fuming; Luo, Wanwei; Luo, Yunjie; Jian, Zhongbao; Gong, Dirong; Polymer Chemistry 11 (2020) 2034–2043; doi:10.1039/C9PY01808E

data_1557270
_publ_section_title
;
 Synthesis and properties investigation of hydroxyl functionalized
 polyisoprene prepared by cobalt catalyzed co-polymerization of isoprene
 and hydroxylmyrcene
;
_journal_issue                   12
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2034
_journal_page_last               2043
_journal_paper_doi               10.1039/C9PY01808E
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C17 H30 Cl2 Co N3 O3 P'
_chemical_formula_sum            'C17 H30 Cl2 Co N3 O3 P'
_chemical_formula_weight         485.24
_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   mixed
_audit_creation_date             2017-11-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-12-10 deposited with the CCDC.	2020-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.858(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5582(3)
_cell_length_b                   8.70090(10)
_cell_length_c                   16.7290(3)
_cell_measurement_reflns_used    5722
_cell_measurement_temperature    296
_cell_measurement_theta_max      73.7900
_cell_measurement_theta_min      5.7070
_cell_volume                     2236.90(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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     42.00  88.00   0.50    0.50    --    0.00  38.00-180.00   92
  2  \w    -60.00 -35.00   0.50    0.50    --    0.00 -38.00 -90.00   50
  3  \w    -15.00  29.00   0.50    0.50    --    0.00  38.00  60.00   88
  4  \w    -86.00  22.00   0.50    0.50    --    0.00 -57.00-180.00  216
  5  \w     59.00  84.00   0.50    0.50    --    0.00  38.00  60.00   50
  6  \w     44.00 119.00   0.50    1.98    --   95.20 -61.00-150.00  150
  7  \w     64.00 109.00   0.50    1.98    --   95.20 -30.00-120.00   90
  8  \w     79.00 154.00   0.50    1.98    --   95.20  30.00-150.00  150
  9  \w     52.00 118.00   0.50    1.98    --   95.20 -82.00-150.00  132
 10  \w     72.00 161.00   0.50    1.98    --   95.20  15.00 -30.00  178
 11  \w      9.00 111.00   0.50    1.98    --   95.20 -61.00  60.00  204
 12  \w    147.00 175.00   0.50    1.98    --   95.20  15.00  30.00   56
 13  \w     80.00 106.00   0.50    1.98    --   95.20  15.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0552609000
_diffrn_orient_matrix_UB_12      -0.0705689000
_diffrn_orient_matrix_UB_13      -0.0879342000
_diffrn_orient_matrix_UB_21      0.0681814000
_diffrn_orient_matrix_UB_22      0.0523403000
_diffrn_orient_matrix_UB_23      -0.0366520000
_diffrn_orient_matrix_UB_31      0.0485280000
_diffrn_orient_matrix_UB_32      -0.1536160000
_diffrn_orient_matrix_UB_33      0.0278930000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11707
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.093
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
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    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4399
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0446P)^2^+0.3559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3744
_reflns_number_total             4399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py01808e2.cif
_cod_data_source_block           lwx-1-1
_cod_depositor_comments
;Adding full bibliography for 1557270.cif.

 Adding full bibliography for 1557270.cif.
;
_cod_database_code               1557270
_reflns_odcompleteness_completeness 99.88
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 C17-H1
 1.901768 with sigma of 0.02
 Co1-H1
 2.759685 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C5(H5), C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              99896
_shelx_shelxl_version_number     2016/6
_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 5.549
_oxdiff_exptl_absorpt_empirical_full_min 0.581