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_4089484
_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 H59 B F24 Ni O2 P2'
_chemical_formula_weight         1327.47
_chemical_name_common            'B6 in manuscript'
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.8623(15)
_cell_length_b                   24.459(2)
_cell_length_c                   25.783(2)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.62
_cell_measurement_theta_min      2.30
_cell_volume                     11895.1(16)
_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 CCD'
_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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            97690
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.9662
_exptl_absorpt_correction_T_min  0.9295
_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    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         8004
_refine_ls_number_restraints     1559
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+24.8011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                5536
_reflns_number_total             8004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400262b_si_002.cif
_cod_data_source_block           lw11
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' 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        11895.4(18)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4089484