Copolymerization of Ethylene with Acrylate Monomers by Amide-Functionalized α-Diimine Pd Catalysts
Zhai, Feng; Solomon, Joseph B.; Jordan, Richard F.; Organometallics 36 (2017) 1873–; doi:10.1021/acs.organomet.7b00209

data_4087340
_publ_section_title
;
 Copolymerization of Ethylene with Acrylate Monomers by
 Amide-Functionalized \a-Diimine Pd Catalysts
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1873
_journal_paper_doi               10.1021/acs.organomet.7b00209
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C48 H47 Cl2 N3 O Pd, 2(C2 H2 Cl4)'
_chemical_formula_sum            'C52 H51 Cl10 N3 O Pd'
_chemical_formula_weight         1194.86
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.547(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5758(18)
_cell_length_b                   14.2713(12)
_cell_length_c                   18.9212(15)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.37
_cell_volume                     5256.5(8)
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            106577
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.452
_diffrn_reflns_theta_min         2.373
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0697 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.9386.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         10817
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0953
_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^)+(0.0130P)^2^+91.7620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8835
_reflns_number_total             10817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00209_si_003.cif
_cod_data_source_block           0289_feng
_cod_database_code               4087340
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.840
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-C52 = C52X-C51X
 1.45 with sigma of 0.02
 C50X-C49X
 1.45 with sigma of 0.02
 Cl5X-Cl6X
 3 with sigma of 0.02
 Cl3X-Cl4X
 3 with sigma of 0.02
 Cl5X-C49X = Cl6X-C49X = Cl3X-C50X = Cl4X-C50X
 1.75 with sigma of 0.02
 C52-C51
 1.45 with sigma of 0.02
 C52-C51 = C52X-C51X
 1.45 with sigma of 0.02
 Cl7X-C52X \\sim Cl7-C52 \\sim Cl8-C52 \\sim Cl8X-C52X \\sim Cl1X-C51X \\sim
Cl10-C51 \\sim Cl9X-C51X
 \\sim Cl9-C51
 with sigma of 0.02
 C51-C52 \\sim C52X-C51X
 with sigma of 0.02
 Cl8X-C52X \\sim Cl8-C52 \\sim Cl7X-C52X \\sim Cl7-C52 \\sim Cl9-C51 \\sim
Cl9X-C51X \\sim Cl1X-C51X ~
 Cl10-C51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl5X) = Uanis(Cl5)
Uanis(C49X) = Uanis(C49)
Uanis(Cl6X) = Uanis(Cl6)
4. Rigid body (RIGU) restrains
 Cl1X, Cl7X, Cl8X, Cl9X, C51X, C52X, Cl7, Cl8, Cl9, Cl10, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3X, Cl4X, C50X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5X, C49X, Cl6X, C50X, Cl3X, Cl4X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5, C49, Cl4, Cl3, C50, Cl6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl1X)=Sof(Cl7X)=Sof(Cl8X)=Sof(Cl9X)=Sof(C51X)=Sof(H51X)=Sof(C52X)=
 Sof(H52X)=1-FVAR(1)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(Cl10)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=
 FVAR(1)
 Sof(Cl3X)=Sof(Cl4X)=Sof(Cl5X)=Sof(Cl6X)=Sof(C49X)=Sof(H49X)=Sof(C50X)=
 Sof(H50X)=1-FVAR(2)
 Sof(Cl6)=Sof(Cl4)=Sof(Cl5)=Sof(Cl3)=Sof(C50)=Sof(H50)=Sof(C49)=Sof(H49)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C21(H21), C40(H40), C51(H51), C52(H52), C51X(H51X), C52X(H52X),
 C50(H50), C49(H49), C49X(H49X), C50X(H50X)
6.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C42(H42),
 C43(H43), C44(H44)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              62271
_shelx_hkl_checksum              21893
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'