Living (co)polymerization of ethylene and bio-based furfuryl acrylate using dibenzobarrelene derived α-diimine palladium catalysts
Du, Cheng; Zhong, Liu; Gao, Jie; Zhong, Shuhuang; Liao, Heng; Gao, Haiyang; Wu, Qing; Polymer Chemistry 10 (2019) 2029–; doi:10.1039/C9PY00126C

data_1550752
_publ_section_title
;
 Living (co)polymerization of ethylene and bio-based furfuryl acrylate
 using dibenzobarrelene derived \a-diimine palladium catalysts
;
_journal_issue                   16
_journal_name_full               'Polymer Chemistry'
_journal_page_first              2029
_journal_paper_doi               10.1039/C9PY00126C
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C49 H53 N2 O3 Pd, C32 H12 B F24'
_chemical_formula_sum            'C81 H65 B F24 N2 O3 Pd'
_chemical_formula_weight         1687.17
_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
_audit_creation_date             2018-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2019-01-28 deposited with the CCDC.    2019-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.474(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.646(2)
_cell_length_b                   21.9906(11)
_cell_length_c                   25.7467(16)
_cell_measurement_reflns_used    7040
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.9690
_cell_measurement_theta_min      3.6320
_cell_volume                     15652.2(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00 -71.00   1.00   35.39    --  -12.91 178.00  30.00   27
  2  \w    -21.00  40.00   1.00   35.39    --  -12.91  77.00   0.00   61
  3  \w    -55.00  -1.00   1.00   35.39    --   13.92 -77.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0051120000
_diffrn_orient_matrix_UB_12      -0.0240267000
_diffrn_orient_matrix_UB_13      -0.0174943000
_diffrn_orient_matrix_UB_21      0.0248870000
_diffrn_orient_matrix_UB_22      0.0077900000
_diffrn_orient_matrix_UB_23      0.0007950000
_diffrn_orient_matrix_UB_31      0.0035526000
_diffrn_orient_matrix_UB_32      -0.0200502000
_diffrn_orient_matrix_UB_33      0.0212707000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49391
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.244
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             6811
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.643
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2151
_refine_ls_number_reflns         28441
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          11.250
_refine_ls_shift/su_mean         0.087
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+36.9799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16786
_reflns_number_total             28441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9py00126c2.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2019-08-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1550751--1550752.cif.
;
_cod_original_cell_volume        15652.3(17)
_cod_original_formula_moiety
'C49 H53 N2 O3 Pd, C48.5 H48.2 N2 O2.5 Pd, C32 H12 B F24, C32 H12 B F23.5, 0.25(F)'
_cod_original_formula_sum        'C162 H127 B2 F47.75 N4 O5.50 Pd2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     3359.34
_cod_database_code               1550752
_chemical_oxdiff_formula         'C H Cl Pd'
_chemical_oxdiff_usercomment     C1b-VFM
_reflns_odcompleteness_completeness 90.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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
 C063-C05O
 3 with sigma of 0.02
 O062-C43
 3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C06C) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C06A) \\sim Ueq,
Uanis(C060) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C06D) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F0AA) = Uanis(F05G) = Uanis(F05I) = Uanis(F05H) = Uanis(F1AA) =
Uanis(F02K)
Uanis(F03U) = Uanis(F00I) = Uanis(F00H)
Uanis(F04H) = Uanis(F05V) = Uanis(F05W) = Uanis(F044) = Uanis(F2) = Uanis(F04G)
Uanis(F05Q) = Uanis(F05P) = Uanis(F05S) = Uanis(F05R) = Uanis(F04D) =
Uanis(F04C)
Uanis(F5) = Uanis(F34) = Uanis(F4)
Uanis(C17) = Uanis(C8)
4. Others
 Fixed Sof: F02K(0.5) F02R(0.5) F042(0.5) F044(0.5) F04C(0.6) F04G(0.5)
 F04K(0.5) F04M(0.5) F04W(0.5) F050(0.5) F05C(0.5) F05G(0.5) F05H(0.5)
 F05K(0.5) F05N(0.5) F05P(0.6) F05R(0.5) F05V(0.5) O05W(0.5) O062(0.5)
 C063(0.4) C06A(0.5) C06B(0.5) H06D(0.5) H06E(0.5) C06C(0.5) C06D(0.5) F5(0.25)
 F05S(0.5) F05Q(0.4) F04D(0.4) F05O(0.5) F05D(0.5) F0(0.5) F02S(0.5) F04N(0.5)
 F1(0.5) F0AA(0.5) F05I(0.5) F1AA(0.5) F04L(0.5) F04X(0.5) F05L(0.5) F05W(0.5)
 F04H(0.5) F2(0.5) F2AA(0.5) C17(0.5) C8(0.5) O1(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 C1AA(0.5) C3(0.5) C4(0.5) C43(0.5) C10(0.6) H10A(0.6) H10B(0.6) F7(0.5)
 F34(0.5)
5.a Ternary CH refined with riding coordinates:
 C013(H013), C016(H016), C01S(H01S), C026(H026), C028(H028), C02B(H02B),
 C031(H031), C033(H033), C03K(H03K), C03N(H03N), C04O(H04O), C055(H055)
5.b Secondary CH2 refined with riding coordinates:
 C02V(H02A,H02D), C03W(H03M,H03O), C06B(H06D,H06E), C1(H1A,H1B), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00P(H00P), C00W(H00W), C00Z(H00Z), C011(H011), C012(H012),
 C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G), C01I(H01I), C01L(H01L),
 C01M(H01M), C01N(H01N), C01T(H01T), C020(H020), C022(H022), C023(H023),
 C029(H029), C02A(H02E), C02C(H02C), C02D(H02G), C02F(H02F), C02J(H02J),
 C02M(H02M), C02N(H02N), C02T(H02T), C02X(H02X), C02Y(H02Y), C030(H030),
 C035(H035), C037(H037), C039(H039), C03A(H03A), C03I(H03I), C03O(H03P),
 C040(H040), C041(H041), C043(H043), C045(H045), C047(H047), C04B(H04B),
 C04E(H04E), C04H(H04H), C04I(H04R), C04P(H04P), C04U(H04U), C04X(H04X),
 C04Y(H04Y), C04Z(H04Z), C052(H052), C053(H053), C056(H056), C057(H057),
 C058(H058), C059(H059), C05A(H05Y), C05I(H05Z)
5.d Idealised Me refined as rotating group:
 C036(H03E,H03F,H03G), C038(H03H,H03J,H03L), C03X(H03B,H03C,H03D), C04D(H04A,
 H04C,H04D), C04J(H04F,H04G,H04I), C04Q(H04J,H04K,H04L), C04T(H04M,H04N,H04Q),
 C051(H05A,H05B,H05C), C05E(H05S,H05T,H05U), C05J(H05D,H05E,H05F), C05L(H05G,
 H05H,H05I), C05S(H05V,H05W,H05X), C05T(H05J,H05K,H05L), C05U(H05M,H05N,H05O),
 C05X(H05P,H05Q,H05R), C061(H06A,H06B,H06C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.862