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_4087339
_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
'C57 H80 N6 O2 Pd2, 2(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C61 H84 Cl4 F6 N6 O8 Pd2 S2'
_chemical_formula_weight         1562.06
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.408(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5396(8)
_cell_length_b                   20.2487(10)
_cell_length_c                   25.5041(13)
_cell_measurement_reflns_used    9056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      2.42
_cell_volume                     7866.5(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.982
_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  0.0742
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            84906
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0669 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.8986.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       plate
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         15907
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+12.8697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9967
_reflns_number_total             15907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00209_si_005.cif
_cod_data_source_block           0222_feng_sq
_cod_database_code               4087339
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.837
_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. Restrained distances
 F3-C59 = F1-C59 = F2-C59
 1.33 with sigma of 0.01
 F2A-C59A = F1A-C59A = F3A-C59A
 1.33 with sigma of 0.005
 F4-C58
 1.33 with sigma of 0.01
 S2-C58A \\sim S2-C58
 with sigma of 0.02
 F4-C58 \\sim F5-C58 \\sim F6-C58 \\sim F4A-C58A \\sim F6A-C58A \\sim F5A-C58A
 with sigma of 0.02
 Cl2A-C60A \\sim Cl1A-C60A \\sim Cl1-C60 \\sim Cl2-C60
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C59) = Uanis(C59A)
Uanis(S1A) = Uanis(S1)
Uanis(F1A) = Uanis(F1)
Uanis(F2A) = Uanis(F2)
Uanis(F3) = Uanis(F3A)
Uanis(O3A) = Uanis(O3)
Uanis(O5A) = Uanis(O5)
Uanis(O4A) = Uanis(O4)
Uanis(F5A) = Uanis(F5)
Uanis(F6A) = Uanis(F6)
Uanis(F4A) = Uanis(F4)
Uanis(C58A) = Uanis(C58)
Uanis(C60A) = Uanis(C60)
Uanis(Cl1) = Uanis(Cl1A)
Uanis(Cl2A) = Uanis(Cl2)
4. Same fragment restrains
{S1, F1, F2, F3, O3, O4, O5, C59} sigma for 1-2: 0.01, 1-3: 0.02
as
{S1A, F1A, F2A, F3A, O3A, O4A, O5A, C59A}
5. Others
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(C59A)=1-
 FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(C59)=FVAR(1)
 Sof(C58)=Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(2)
 Sof(C58A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(2)
 Sof(Cl1A)=Sof(C60A)=Sof(H60C)=Sof(H60D)=Sof(Cl2A)=1-FVAR(3)
 Sof(Cl1)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(Cl2)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C20(H20), C29(H29), C32(H32), C39(H39), C52(H52)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C61(H61A,H61B), C60(H60A,H60B), C60A(H60C,H60D)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24), C34(H34),
 C35(H35), C36(H36), C48(H48), C49(H49), C50(H50)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C45(H45A,
 H45B,H45C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C)
;
_shelx_res_checksum              45029
_shelx_hkl_checksum              72387
_shelx_fab_checksum              39927
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'