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_7048364
_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
'C44 H60 F6 N5 O4 P2 Pd S2 Zn, C2 F6 N O4 S2, C4 H8 O'
_chemical_formula_sum            'C50 H68 F12 N6 O9 P2 Pd S4 Zn'
_chemical_formula_weight         1487.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-08-17
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2017-08-17 deposited with the CCDC.
2018-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0449(7)
_cell_length_b                   14.2330(7)
_cell_length_c                   29.2644(13)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.66
_cell_measurement_theta_min      2.48
_cell_volume                     6246.4(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi layer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            71133
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.95
_diffrn_reflns_theta_min         1.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1230 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.8758.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         18553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+2.1750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                15713
_reflns_number_total             18553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt03777a3.cif
_cod_data_source_block           a17_a35sad
_cod_depositor_comments
'Adding full bibliography for 7048364--7048366.cif.'
_cod_database_code               7048364
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C37(H37), C25(H25), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C28(H28A,H28B), C26(H26A,H26B), C39(H39A,H39B), C18(H18A,
 H18B), C33(H33A,H33B), C30(H30A,H30B), C7(H7A,H7B), C29(H29A,H29B), C20(H20A,
 H20B), C41(H41A,H41B), C40(H40A,H40B), C34(H34A,H34B), C21(H21A,H21B),
 C32(H32A,H32B), C6(H6A,H6B), C27(H27A,H27B), C35(H35A,H35B), C42(H42A,H42B),
 C24(H24A,H24B), C36(H36A,H36B), C22(H22A,H22B), C38(H38A,H38B), C43(H43A,H43B),
  C46(H46A,H46B), C45(H45A,H45B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C4(H4), C13(H13), C10(H10), C11(H11), C2(H2), C14(H14),
 C16(H16), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'