Enhancement on Alternating Copolymerization of Carbon Monoxide and Styrene by Dibenzobarrelene-Based α-Diimine Palladium Catalysts
Xiao, Zefan; Zheng, Handou; Du, Cheng; Zhong, Liu; Liao, Heng; Gao, Jie; Gao, Haiyang; Wu, Qing; Macromolecules 51 (2018) 9110–; doi:10.1021/acs.macromol.8b01786

data_1552817
_publ_section_title
;
 Enhancement on Alternating Copolymerization of Carbon Monoxide and
 Styrene by Dibenzobarrelene-Based \a-Diimine Palladium Catalysts
;
_journal_issue                   22
_journal_name_full               Macromolecules
_journal_page_first              9110
_journal_paper_doi               10.1021/acs.macromol.8b01786
_journal_volume                  51
_journal_year                    2018
_chemical_formula_moiety         'C31 H31 Cl N2 O6 Pd, C H2 Cl2'
_chemical_formula_sum            'C32 H33 Cl3 N2 O6 Pd'
_chemical_formula_weight         754.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                79.358(2)
_cell_angle_beta                 68.593(2)
_cell_angle_gamma                84.171(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1018(2)
_cell_length_b                   12.1188(2)
_cell_length_c                   12.3413(3)
_cell_measurement_reflns_used    13180
_cell_measurement_temperature    158.54(10)
_cell_measurement_theta_max      73.6170
_cell_measurement_theta_min      3.7137
_cell_volume                     1654.96(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      158.54(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.967
_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    -58.00 -11.00   1.00    1.00    --  -40.84 -57.00   0.00   47
  2  \w    -67.00  35.00   1.00    1.00    --  -40.84  37.00 150.00  102
  3  \w      7.00  32.00   1.00    1.00    --   44.00  87.00 161.71   25
  4  \w     13.00  38.00   1.00    1.00    --   48.00  81.00 135.43   25
  5  \w     27.00  53.00   1.00    1.00    --   60.00  76.00 124.88   26
  6  \w     32.00  62.00   1.00    1.00    --   64.00  76.00  85.74   30
  7  \w     92.00 143.00   1.00    1.00    --   64.00  77.00  25.72   51
  8  \w     98.00 135.00   1.00    1.00    --   60.00  77.00 -27.15   37
  9  \w     94.00 173.00   1.00    3.00    --  108.22 125.00   0.00   79
 10  \w    124.00 151.00   1.00    3.00    --  108.22  77.00 -30.00   27
 11  \w    140.00 168.00   1.00    3.00    --  108.22  61.00-150.00   28
 12  \w    115.00 140.00   1.00    1.00    --   68.00  76.00-164.77   25
 13  \w    111.00 174.00   1.00    3.00    --  108.22  77.00-180.00   63
 14  \w     75.00 103.00   1.00    3.00    --  108.22  77.00-120.00   28
 15  \w     78.00 171.00   1.00    3.00    --  108.22  61.00-120.00   93
 16  \w     79.00 106.00   1.00    3.00    --  108.22  61.00 -30.00   27
 17  \w     78.00 107.00   1.00    3.00    --  108.22  61.00 -60.00   29
 18  \w     79.00 160.00   1.00    3.00    --  108.22  61.00   0.00   81
 19  \w    120.00 176.00   1.00    3.00    --  108.22  77.00  90.00   56
 20  \w     87.00 137.00   1.00    1.00    --   64.00  77.00 158.32   50
 21  \w     80.00 107.00   1.00    3.00    --  108.22  61.00  90.00   27
 22  \w     79.00 117.00   1.00    3.00    --  108.22  61.00 120.00   38
 23  \w     76.00 156.00   1.00    3.00    --  108.22  77.00 150.00   80
 24  \w     78.00 104.00   1.00    3.00    --  108.22  61.00  30.00   26
 25  \w     75.00 102.00   1.00    3.00    --  108.22  77.00  90.00   27
 26  \w     76.00 160.00   1.00    3.00    --  108.22  77.00 120.00   84
 27  \w     75.00 117.00   1.00    3.00    --  108.22  77.00  30.00   42
 28  \w     75.00 101.00   1.00    3.00    --  108.22  77.00 -30.00   26
 29  \w     75.00 177.00   1.00    3.00    --  108.22  77.00 -60.00  102
 30  \w     79.00 107.00   1.00    3.00    --  108.22  61.00-150.00   28
 31  \w     76.00 102.00   1.00    3.00    --  108.22  77.00-150.00   26
 32  \w     76.00 102.00   1.00    3.00    --  108.22  77.00-180.00   26
 33  \w     78.00 153.00   1.00    3.00    --  108.22  61.00 -90.00   75
 34  \w     75.00 169.00   1.00    3.00    --  108.22  77.00  60.00   94
 35  \w     79.00 104.00   1.00    3.00    --  108.22  61.00 150.00   25
 36  \w     30.00  72.00   1.00    1.00    --   64.00  77.00  25.72   42
 37  \w     31.00  59.00   1.00    1.00    --   64.00  76.00 -15.40   28
 38  \w     26.00  52.00   1.00    1.00    --   60.00  77.00 -27.15   26
 39  \w     18.00  45.00   1.00    1.00    --   52.00  80.00 -72.72   27
 40  \w     34.00  87.00   1.00    1.00    --   64.00  75.00 -98.64   53
 41  \w     35.00  70.00   1.00    1.00    --   68.00  76.00-164.77   35
 42  \w     31.00  86.00   1.00    1.00    --   64.00  76.00-133.43   55
 43  \w      6.00  31.00   1.00    1.00    --   44.00  89.00-161.45   25
 44  \w      6.00  32.00   1.00    1.00    --   44.00  90.00   9.55   26
 45  \w     22.00  47.00   1.00    1.00    --   56.00  78.00  81.44   25
 46  \w     30.00  66.00   1.00    1.00    --   64.00  77.00 158.32   36
 47  \w     34.00 139.00   1.00    3.00    --  108.22 -61.00 -30.00  105
 48  \w     78.00 109.00   1.00    3.00    --  108.22 -94.00  30.00   31
 49  \w     45.00 118.00   1.00    3.00    --  108.22-125.00-120.00   73
 50  \w     33.00 104.00   1.00    3.00    --  108.22-125.00-180.00   71
 51  \w     30.00  98.00   1.00    1.00    --   40.84-125.00-120.00   68
 52  \w     30.00 109.00   1.00    3.00    --  108.22 -94.00 -60.00   79
 53  \w      1.00  83.00   1.00    1.00    --   40.84 -99.00 -30.00   82
 54  \w    -47.00 -11.00   1.00    1.00    --  -40.84 -57.00-180.00   36
 55  \w    -95.00 -69.00   1.00    1.00    --  -40.84 -57.00-180.00   26
 56  \w   -115.00 -66.00   1.00    1.00    --  -40.84 -57.00   0.00   49
 57  \w   -109.00 -69.00   1.00    1.00    --  -40.84 -37.00  90.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0757344000
_diffrn_orient_matrix_UB_12      0.0684717000
_diffrn_orient_matrix_UB_13      0.0970098000
_diffrn_orient_matrix_UB_21      -0.0435289000
_diffrn_orient_matrix_UB_22      -0.1098162000
_diffrn_orient_matrix_UB_23      0.0850578000
_diffrn_orient_matrix_UB_31      0.1053169000
_diffrn_orient_matrix_UB_32      -0.0024291000
_diffrn_orient_matrix_UB_33      0.0424290000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21624
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.720
_diffrn_reflns_theta_min         3.714
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0790P)^2^+1.9610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6060
_reflns_number_total             6468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma8b01786_si_005.cif
_cod_data_source_block           1
_cod_database_code               1552817
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         PdCNOClH
_chemical_oxdiff_usercomment     N7
_reflns_odcompleteness_completeness 99.00
_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. Restrained distances
 Pd1-Cl1A
 2.3 with sigma of 0.02
 Pd1-C1A
 1.9 with sigma of 0.02
 Pd1-Cl1
 2.3 with sigma of 0.02
 Pd1-C1
 1.9 with sigma of 0.02
 Cl0A-C0AA
 1.6 with sigma of 0.02
 Cl2A-C0AA
 1.6 with sigma of 0.02
 Cl2A-Cl0A
 2.8 with sigma of 0.02
 Cl3-C33
 1.65 with sigma of 0.02
 C33-Cl2
 1.65 with sigma of 0.02
 Cl7-Cl3A
 2.8 with sigma of 0.02
 Cl3A-C1AA
 1.65 with sigma of 0.02
 C1AA-Cl7
 1.65 with sigma of 0.02
 Cl3A-Cl7
 2.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl0A) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(Cl2A) \\sim Ueq,
Uanis(Cl0A) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(Cl2A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(Cl7) \\sim Ueq, Uanis(Cl3A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl7) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(Cl3A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(Cl1) = Uanis(Cl1A) = Uanis(C1)
4. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(2)
 Fixed Sof: C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) Cl3(0.5) Cl2(0.5) C33(0.5) H33A(0.5) H33B(0.5) Cl0A(0.25)
 Cl2A(0.25) C0AA(0.25) H0AA(0.25) H0AB(0.25) Cl3A(0.25) Cl7(0.25) C1AA(0.25)
 H1AD(0.25) H1AE(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C0AA(H0AA,H0AB), C1AA(H1AD,H1AE)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C13(H13), C25(H25), C12(H12), C29(H29), C7(H7), C11(H11), C8(H8),
 C9(H9), C15(H15)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C30(H30A,H30B,
 H30C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C1(H1A,
 H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_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 2.040
_oxdiff_exptl_absorpt_empirical_full_min 0.513