Mechanistic Details of the Nickel-Mediated Formation of Acrylates from CO2, Ethylene and Methyl Iodide
Plessow, Philipp N.; Weigel, Laura; Lindner, Ronald; Schäfer, Ansgar; Rominger, Frank; Limbach, Michael; Hofmann, Peter; Organometallics 32 (2013) 3327–; doi:10.1021/om400262b

data_4089483
_publ_section_title
;
 Mechanistic Details of the Nickel-Mediated Formation of Acrylates from
 CO2, Ethylene and Methyl Iodide
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3327
_journal_paper_doi               10.1021/om400262b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C54.5 H60 B Cl F24 Ni O2 P2'
_chemical_formula_weight         1369.93
_chemical_name_common            'B1 in manuscript'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.864(3)
_cell_angle_beta                 86.826(3)
_cell_angle_gamma                74.241(3)
_cell_formula_units_Z            4
_cell_length_a                   12.9017(14)
_cell_length_b                   20.347(2)
_cell_length_c                   25.577(3)
_cell_measurement_reflns_used    4539
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.27
_cell_measurement_theta_min      2.19
_cell_volume                     6100.6(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'ImuS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_sigmaI/netI    0.1489
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54200
_diffrn_reflns_theta_full        21.04
_diffrn_reflns_theta_max         21.04
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2796
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1790
_refine_ls_number_reflns         13150
_refine_ls_number_restraints     8189
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1651
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^2^+6.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2290
_reflns_number_gt                6687
_reflns_number_total             13150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400262b_si_002.cif
_cod_data_source_block           lw16
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        6100.5(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C54.50 H60 B Cl F24 Ni O2 P2'
_cod_database_code               4089483