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_1552820
_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 H27 Cl N2 O2 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C33 H31 Cl5 N2 O2 Pd'
_chemical_formula_weight         771.25
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.976(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9080(7)
_cell_length_b                   22.0742(18)
_cell_length_c                   15.5558(14)
_cell_measurement_reflns_used    7645
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      54.98
_cell_measurement_theta_min      6.14
_cell_volume                     3350.8(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31798
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies,'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.853
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+2.9230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                5921
_reflns_number_total             7645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma8b01786_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               1552820
_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:
 C25(H25), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C3(H3), C4(H4), C30(H30), C13(H13), C11(H11), C23(H23), C7(H7),
 C27(H27), C20(H20), C10(H10), C6(H6), C29(H29), C28(H28), C21(H21), C22(H22)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'