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_1552818
_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         'C35 H35 Cl N2 O6 Pd, C H2 Cl2'
_chemical_formula_sum            'C36 H37 Cl3 N2 O6 Pd'
_chemical_formula_weight         806.43
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7312(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3985(2)
_cell_length_b                   20.1081(5)
_cell_length_c                   13.8378(3)
_cell_measurement_reflns_used    7830
_cell_measurement_temperature    150.08(10)
_cell_measurement_theta_max      66.8710
_cell_measurement_theta_min      3.8550
_cell_volume                     3445.99(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      150.08(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5058
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -22.00   55.00   1.0000    1.5950
omega____ theta____ kappa____ phi______ frames
    -       40.7938  -38.0000    0.0000 77

  2 omega   16.00   56.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 40

  3 omega   20.00   61.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 41

  4 omega   46.00   78.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   90.0000 32

  5 omega   23.00   66.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 43

  6 omega   94.00  168.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000    0.0000 74

  7 omega   29.00   71.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 42

  8 omega   27.00  120.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -90.0000 93

  9 omega   25.00   90.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -126.0000 -180.0000 65

 10 omega   12.00   75.00   1.0000    6.3850
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -180.0000 63

 11 omega   15.00  117.00   1.0000    1.5950
omega____ theta____ kappa____ phi______ frames
    -       40.7938   38.0000 -180.0000 102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0808960000
_diffrn_orient_matrix_UB_12      -0.0495105000
_diffrn_orient_matrix_UB_13      -0.0411564000
_diffrn_orient_matrix_UB_21      0.0935476000
_diffrn_orient_matrix_UB_22      0.0476570000
_diffrn_orient_matrix_UB_23      0.0285651000
_diffrn_orient_matrix_UB_31      0.0134572000
_diffrn_orient_matrix_UB_32      -0.0339465000
_diffrn_orient_matrix_UB_33      0.0995088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14285
_diffrn_reflns_theta_full        67.03
_diffrn_reflns_theta_max         67.03
_diffrn_reflns_theta_min         4.19
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_length       0.500
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_exptl_crystal_size_rad          0.080
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+1.2855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                5351
_reflns_number_total             6033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma8b01786_si_004.cif
_cod_data_source_block           12097a
_cod_original_cell_volume        3445.99(12)
_cod_database_code               1552818
_chemical_oxdiff_formula         'C20 H20 N2 O2 Pt Cl'
_chemical_oxdiff_usercomment     'XZF plate red 0.32 0.31 0.04 150K'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.28
_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:
 C1DA(H1DA), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C5AA(H5AA), C10(H10), C8BA(H8BA), C7CA(H7CA), C2DA(H2DA),
 C4DA(H4DA), C6(H6), C1(H1), C11(H11), C9(H9), C14(H14)
2.d Idealised Me refined as rotating group:
 C3BA(H3BA,H3BB,H3BC), C7BA(H7BA,H7BB,H7BC), C30(H30A,H30B,H30C), C5(H5A,H5B,
 H5C), C12(H12A,H12B,H12C), C2AA(H2AA,H2AB,H2AC)
;
_olex2_submission_special_instructions 'No special instructions were received'