Investigations on the catalytic carboxylation of olefins with CO2 towards α,β-unsaturated carboxylic acid salts: characterization of intermediates and ligands as well as substrate effects.
Jevtovikj, Ivana; Manzini, Simone; Hanauer, Matthias; Rominger, Frank; Schaub, Thomas; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11083–11094; doi:10.1039/c5dt01040c

data_7034853
_publ_section_title
;
 Investigations on the catalytic carboxylation of olefins with CO2 towards
 \a,\b-unsaturated carboxylic acid salts: characterization of
 intermediates and ligands as well as substrate effects.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11083
_journal_page_last               11094
_journal_paper_doi               10.1039/c5dt01040c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C34 H56 Ni P2'
_chemical_formula_weight         585.43
_chemical_name_common            '2b in manuscript'
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-03-05 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.564(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6643(18)
_cell_length_b                   9.5838(16)
_cell_length_c                   31.345(6)
_cell_measurement_reflns_used    3098
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.47
_cell_volume                     3175.7(10)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17547
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_min         1.926
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.7686
_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            orange
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0584
_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^)+3.9910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4308
_reflns_number_total             5635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01040c2.cif
_cod_data_source_block           ij5
_cod_depositor_comments
'Adding full bibliography for 7034853--7034856.cif.'
_cod_original_cell_volume        3175.7(9)
_cod_database_code               7034853
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.898
_shelxl_version_number           2013-4
_shelx_res_checksum              84898