Indole-bridged bisphosphine-monoxide palladium catalysts for ethylene polymerization and copolymerization with polar monomers
Li, Kangkang; Ye, Junhao; Wang, Zhen; Mu, Hongliang; Jian, Zhongbao; Polymer Chemistry 11 (2020) 2740–2748; doi:10.1039/D0PY00100G

data_1557623
_publ_section_title
;
 Indole-bridged bisphosphine-monoxide palladium catalysts for ethylene
 polymerization and copolymerization with polar monomers
;
_journal_issue                   15
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2740
_journal_page_last               2748
_journal_paper_doi               10.1039/D0PY00100G
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C27 H34 Cl N3 O3 P2 Pd, C H Cl3'
_chemical_formula_sum            'C28 H35 Cl4 N3 O3 P2 Pd'
_chemical_formula_weight         771.73
_chemical_properties_physical    Deliquescent,Heat-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2020-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                67.146(2)
_cell_angle_beta                 74.271(2)
_cell_angle_gamma                78.535(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2563(6)
_cell_length_b                   12.7674(7)
_cell_length_c                   14.3032(8)
_cell_measurement_reflns_used    8804
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.010
_cell_measurement_theta_min      3.778
_cell_volume                     1813.12(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10880
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        59.010
_diffrn_reflns_theta_max         59.010
_diffrn_reflns_theta_min         3.778
_exptl_absorpt_coefficient_mu    7.930
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1038 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.6949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.796
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5023
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0731P)^2^+11.6171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4789
_reflns_number_total             5023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py00100g2.cif
_cod_data_source_block           191024pd7_0m_sq
_cod_depositor_comments
;Adding full bibliography for 1557622--1557624.cif.

 Adding full bibliography for 1557622--1557624.cif.
;
_cod_database_code               1557623
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.162
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C0, Cl1}
{Cl0, C0'}
3. Uiso/Uaniso restraints and constraints
Pd1 \\sim C0 \\sim Cl0 \\sim C0' \\sim Cl1: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C0) = Uanis(Cl1)
Uanis(Cl0) = Uanis(C0')
4. Others
 Sof(C0')=Sof(H0'A)=Sof(H0'B)=Sof(H0'C)=Sof(Cl1)=1-FVAR(1)
 Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=Sof(Cl0)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C0AA(H0AA)
5.b Me refined with riding coordinates:
 C0(H0A,H0B,H0C), C0'(H0'A,H0'B,H0'C), C00Q(H00A,H00B,H00C), C00V(H00D,H00E,
 H00F), C00Z(H00H,H00I,H00M), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F),
 C012(H01G,H01H,H01I)
5.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00J(H00J), C00K(H00K), C00L(H00L), C00O(H00O), C00P(H00P),
 C00R(H00R), C00T(H00T), C00W(H00W), C00X(H00X), C00Y(H00Y), C013(H013),
 C014(H014)
;
_shelx_res_checksum              46165
_shelx_fab_checksum              87290
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'