Ligand-controlled insertion regioselectivity accelerates copolymerisation of ethylene with methyl acrylate by cationic bisphosphine monoxide‒palladium catalysts
Mitsushige, Yusuke; Carrow, Brad P.; Ito, Shingo; Nozaki, Kyoko; Chem. Sci. 7 (2016) 737–; doi:10.1039/C5SC03361F

data_1540487
_publ_section_title
;
 Ligand-controlled insertion regioselectivity accelerates copolymerisation
 of ethylene with methyl acrylate by cationic bisphosphine
 monoxide--palladium catalysts
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              737
_journal_paper_doi               10.1039/C5SC03361F
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C30 H49 N O3 P2 Pd, F6 P, C H2 Cl2'
_chemical_formula_sum            'C31 H51 Cl2 F6 N O3 P3 Pd'
_chemical_formula_weight         869.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2015-06-25 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;
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_cell_angle_gamma                90
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_cell_length_a                   8.2128(13)
_cell_length_b                   22.725(4)
_cell_length_c                   20.504(4)
_cell_measurement_reflns_used    7644
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.6
_cell_measurement_theta_min      3.1
_cell_volume                     3765.1(12)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto, et al.)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0262
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_diffrn_reflns_laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13465
_diffrn_reflns_point_group_measured_fraction_full 0.955
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
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_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       Block
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_exptl_crystal_size_mid          0.100
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_refine_diff_density_min         -0.438
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_refine_ls_abs_structure_details
;
 Flack x determined using 3034 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7013
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+1.9380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.898
_reflns_friedel_fraction_full    0.912
_reflns_friedel_fraction_max     0.900
_reflns_number_gt                6801
_reflns_number_total             7013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03361f2.cif
_cod_data_source_block           iPMA21Py
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1540485--1540489.cif.
;
_cod_database_code               1540487
_shelx_estimated_absorpt_t_min   0.708
_shelx_estimated_absorpt_t_max   0.960
_shelxl_version_number           2014/6
_shelx_res_checksum              71450