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_1557624
_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         'C37 H44 Cl N O3 P2 Pd, C H Cl3'
_chemical_formula_sum            'C38 H45 Cl4 N O3 P2 Pd'
_chemical_formula_weight         873.89
_chemical_properties_physical    Deliquescent,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     direct
_audit_creation_date             2019-09-23
_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                65.2480(10)
_cell_angle_beta                 83.2000(10)
_cell_angle_gamma                79.8140(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2352(4)
_cell_length_b                   14.3325(5)
_cell_length_c                   14.8170(5)
_cell_measurement_reflns_used    9196
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      59.064
_cell_measurement_theta_min      3.430
_cell_volume                     1940.40(12)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12056
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        59.064
_diffrn_reflns_theta_max         59.064
_diffrn_reflns_theta_min         3.430
_exptl_absorpt_coefficient_mu    7.468
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0943 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.6843.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.249
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0838P)^2^+4.6872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4935
_reflns_number_total             5422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0py00100g2.cif
_cod_data_source_block           190904b_0m_sq
_cod_depositor_comments
;Adding full bibliography for 1557622--1557624.cif.

 Adding full bibliography for 1557622--1557624.cif.
;
_cod_database_code               1557624
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.522
_shelx_estimated_absorpt_t_min   0.317
_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.a Ternary CH refined with riding coordinates:
 C015(H015)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00M(H00M), C00O(H00O), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C011(H011), C012(H012), C014(H014), C018(H018)
2.c Idealised Me refined as rotating group:
 C00C(H00A,H00B,H00C), C010(H01A,H01B,H01C), C016(H01D,H01E,H01F), C017(H01G,
 H01H,H01I), C019(H01J,H01K,H01L), C01A(H01M,H01N,H01O), C01B(H01P,H01Q,H01R),
 C01C(H01S,H01T,H01U), C01D(H01V,H01W,H01X)
;
_shelx_res_checksum              70918
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'