Norbornene homopolymerization and copolymerization with ethylene by phosphine-sulfonate nickel catalysts
Chen, Min; Zou, Wenping; Cai, Zhengguo; Chen, Changle; Polym. Chem. 6 (2015) 2669–; doi:10.1039/C5PY00010F

data_1518681
_publ_section_title
;
 Norbornene homopolymerization and copolymerization with ethylene by
 phosphine-sulfonate nickel catalysts
;
_journal_issue                   14
_journal_name_full               'Polym. Chem.'
_journal_page_first              2669
_journal_paper_doi               10.1039/C5PY00010F
_journal_volume                  6
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C46 H39 B F15 Ni O3 P S'
_chemical_formula_weight         1057.32
_chemical_name_systematic        '[(o-Cy2-PC6H4SO3B(C6F5)3)Ni(allyl)]'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-01-04 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5629(3)
_cell_length_b                   15.6599(2)
_cell_length_c                   11.55970(10)
_cell_measurement_reflns_used    5194
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      69.4468
_cell_measurement_theta_min      3.3442
_cell_volume                     4446.47(9)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Gemini S Ultra, Agilent Technologies'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11103
_diffrn_reflns_point_group_measured_fraction_full 0.704
_diffrn_reflns_point_group_measured_fraction_max 0.693
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.574
_diffrn_reflns_theta_min         3.347
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             2152
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/Hexane'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1350 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(17)
_refine_ls_extinction_coef       0.00029(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         5783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0592P)^2^+0.3055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.337
_reflns_Friedel_fraction_full    0.380
_reflns_Friedel_fraction_max     0.369
_reflns_number_gt                5442
_reflns_number_total             5783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5py00010f2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 1518680--1518681.cif.'
_cod_database_code               1518681
_shelx_estimated_absorpt_t_min   0.484
_shelx_estimated_absorpt_t_max   0.569
_shelxl_version_number           2013-4
_shelx_res_checksum              38463