Highly efficient palladium-catalysed carbon dioxide hydrosilylation employing PMP ligands.
Steinhoff, Patrick; Paul, Melanie; Schroers, Julian P.; Tauchert, Michael E.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1017–1022; doi:10.1039/c8dt03777a

data_7048365
_publ_section_title
;
 Highly efficient palladium-catalysed carbon dioxide hydrosilylation
 employing PMP ligands.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1017
_journal_page_last               1022
_journal_paper_doi               10.1039/c8dt03777a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C42 H60 Li N4 P2 Pd 1+, N1 S2 O4 C2 F6 1-, C7 H8'
_chemical_formula_sum            'C43 H60 F3 Li N4.5 O2 P2 Pd S'
_chemical_formula_weight         936.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-12-14 deposited with the CCDC.
2018-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6156(8)
_cell_length_b                   19.4178(10)
_cell_length_c                   40.0329(19)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.16
_cell_volume                     11219.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Mercury 3.9'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            68052
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.490
_diffrn_reflns_theta_min         1.758
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1512 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.8603.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3900
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         4.098
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         11606
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0784
_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^)+(0.0796P)^2^+113.4898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1889
_refine_ls_wR_factor_ref         0.1976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9620
_reflns_number_total             11606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03777a3.cif
_cod_data_source_block           n17_b46
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048364--7048366.cif.
;
_cod_original_formula_sum        'C43 H60 F3 Li N4.50 O2 P2 Pd S'
_cod_database_code               7048365
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              47657