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_7048366
_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         'C43 H64 N4 O P2 Zn, 2(C2 F6 N O4 S2)'
_chemical_formula_sum            'C47 H64 F12 N6 O9 P2 S4 Zn'
_chemical_formula_weight         1340.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_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_date             2018-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-06 deposited with the CCDC.
2018-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                87.1040(10)
_cell_angle_beta                 89.9450(10)
_cell_angle_gamma                77.8480(10)
_cell_formula_units_Z            4
_cell_length_a                   13.7809(10)
_cell_length_b                   16.7029(12)
_cell_length_c                   26.0578(18)
_cell_measurement_reflns_used    4472
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.43
_cell_measurement_theta_min      2.26
_cell_volume                     5855.8(7)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66902
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1499 before and 0.0533 after correction.
The Ratio of minimum to maximum transmission is 0.8158.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1467
_refine_ls_number_reflns         21767
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0000P)^2^+2.8271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                15888
_reflns_number_total             21767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt03777a3.cif
_cod_data_source_block           m18_a38
_cod_depositor_comments
'Adding full bibliography for 7048364--7048366.cif.'
_cod_database_code               7048366
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2-H2
 0.87 with sigma of 0.01
 O1-H1
 0.87 with sigma of 0.01
 C44-H2
 1.931539 with sigma of 0.02
 Zn2-H2
 2.663034 with sigma of 0.02
 C1-H1
 1.948286 with sigma of 0.02
 Zn1-H1
 2.722138 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C8(H8), C19(H19), C45(H45), C63(H63), C2(H2A), C51(H51), C25(H25), C69(H69)
3.b Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C81(H81A,H81B), C3(H3A,H3B), C10(H10A,H10B), C62(H62A,H62B),
 C9(H9A,H9B), C37(H37A,H37B), C80(H80A,H80B), C46(H46A,H46B), C68(H68A,H68B),
 C54(H54A,H54B), C74(H74A,H74B), C64(H64A,H64B), C55(H55A,H55B), C11(H11A,H11B),
  C38(H38A,H38B), C65(H65A,H65B), C12(H12A,H12B), C7(H7A,H7B), C30(H30A,H30B),
 C28(H28A,H28B), C53(H53A,H53B), C6(H6A,H6B), C56(H56A,H56B), C5(H5A,H5B),
 C24(H24A,H24B), C52(H52A,H52B), C50(H50A,H50B), C73(H73A,H73B), C49(H49A,H49B),
  C20(H20A,H20B), C72(H72A,H72B), C66(H66A,H66B), C22(H22A,H22B), C48(H48A,
 H48B), C29(H29A,H29B), C67(H67A,H67B), C26(H26A,H26B), C4(H4A,H4B), C27(H27A,
 H27B), C71(H71A,H71B), C47(H47A,H47B), C13(H13A,H13B), C23(H23A,H23B),
 C21(H21A,H21B), C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C32(H32), C85(H85), C43(H43), C86(H86), C34(H34), C17(H17),
 C58(H58), C60(H60), C16(H16), C33(H33), C84(H84), C59(H59), C83(H83), C77(H77),
  C42(H42), C76(H76), C78(H78), C40(H40), C41(H41)
3.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'