Reversible Carbon Dioxide Binding by Simple Lewis Base Adducts with Electron-Rich Phosphines.
Buß, Florenz; Mehlmann, Paul; Mück-Lichtenfeld, Christian; Bergander, Klaus; Dielmann, Fabian; Journal of the American Chemical Society 138 (2016) 1840–1843; doi:10.1021/jacs.5b13116

data_4130042
_publ_section_title
;
 Reversible Carbon Dioxide Binding by Simple Lewis Base Adducts with
 Electron-Rich Phosphines.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1840
_journal_page_last               1843
_journal_paper_doi               10.1021/jacs.5b13116
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C50 H94 Cl4 N12 P2 Pd2'
_chemical_formula_sum            'C50 H94 Cl4 N12 P2 Pd2'
_chemical_formula_weight         1279.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                70.7991(7)
_cell_angle_beta                 70.3104(8)
_cell_angle_gamma                88.7659(7)
_cell_formula_units_Z            1
_cell_length_a                   10.7627(2)
_cell_length_b                   11.3637(2)
_cell_length_c                   14.0991(2)
_cell_measurement_reflns_used    7593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.248
_cell_measurement_theta_min      2.594
_cell_volume                     1525.49(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15330
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.259
_diffrn_reflns_theta_min         2.904
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0290 after correction.
The Ratio of minimum to maximum transmission is 0.9211.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.9682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6739
_reflns_number_total             7516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13116_si_004.cif
_cod_data_source_block           compound7
_cod_database_code               4130042
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.034) H4B(0.034) H4C(0.034) H5A(0.049) H5B(0.049) H5C(0.049)
 H6(0.02) H7A(0.032) H7B(0.032) H7C(0.032) H8A(0.042) H8B(0.042) H8C(0.042)
 H9(0.02) H10A(0.04) H10B(0.04) H10C(0.04) H11A(0.037) H11B(0.037) H11C(0.037)
 H15A(0.037) H15B(0.037) H15C(0.037) H16A(0.032) H16B(0.032) H16C(0.032)
 H17(0.02) H18A(0.037) H18B(0.037) H18C(0.037) H19A(0.037) H19B(0.037)
 H19C(0.037) H20(0.021) H21A(0.048) H21B(0.048) H21C(0.048) H22A(0.043)
 H22B(0.043) H22C(0.043) H23(0.019) H24A(0.034) H24B(0.034) H24C(0.034)
 H25A(0.034) H25B(0.034) H25C(0.034)
 Fixed X: H4A(0.619) H4B(0.4653) H4C(0.5762) H5A(0.2772) H5B(0.3229)
 H5C(0.3611) H6(0.8529) H7A(0.9489) H7B(0.8573) H7C(0.8086) H8A(0.7252)
 H8B(0.8553) H8C(0.7139) H9(0.5274) H10A(0.2767) H10B(0.3087) H10C(0.3788)
 H11A(0.4909) H11B(0.392) H11C(0.3411) H15A(0.8628) H15B(0.8314) H15C(0.7136)
 H16A(0.7722) H16B(0.8593) H16C(0.9232) H17(0.6737) H18A(0.5028) H18B(0.5315)
 H18C(0.5859) H19A(0.7758) H19B(0.8864) H19C(0.8109) H20(0.7516) H21A(0.6779)
 H21B(0.6663) H21C(0.5776) H22A(0.9776) H22B(0.9135) H22C(0.9267) H23(0.928)
 H24A(0.9496) H24B(1.0395) H24C(1.0529) H25A(0.7098) H25B(0.8276) H25C(0.7506)
 Fixed Y: H4A(0.2573) H4B(0.2072) H4C(0.1114) H5A(0.2898) H5B(0.2928)
 H5C(0.4116) H6(0.1525) H7A(0.1756) H7B(0.2881) H7C(0.1677) H8A(-0.0431) H8B(-
 0.0405) H8C(-0.0294) H9(0.3041) H10A(0.2044) H10B(0.2295) H10C(0.1245)
 H11A(0.4939) H11B(0.4625) H11C(0.4372) H15A(0.6977) H15B(0.6559) H15C(0.6873)
 H16A(0.3597) H16B(0.4918) H16C(0.3647) H17(0.4945) H18A(0.5397) H18B(0.6476)
 H18C(0.6692) H19A(0.6838) H19B(0.6171) H19C(0.7227) H20(0.1304) H21A(0.181)
 H21B(0.0441) H21C(0.1478) H22A(0.1875) H22B(0.0541) H22C(0.1723) H23(0.1242)
 H24A(0.0559) H24B(0.0109) H24C(0.155) H25A(0.0113) H25B(-0.0769) H25C(-0.0395)
 Fixed Z: H4A(-0.1496) H4B(-0.0878) H4C(-0.083) H5A(0.1386) H5B(0.0173)
 H5C(0.0427) H6(0.0395) H7A(-0.1368) H7B(-0.1336) H7C(-0.1517) H8A(0.1175)
 H8B(0.0188) H8C(0.0042) H9(0.286) H10A(0.3036) H10B(0.3986) H10C(0.3523)
 H11A(0.1652) H11B(0.2861) H11C(0.1995) H15A(0.3629) H15B(0.4893) H15C(0.4426)
 H16A(0.6766) H16B(0.6078) H16C(0.6021) H17(0.2528) H18A(0.3893) H18B(0.2755)
 H18C(0.3616) H19A(0.1335) H19B(0.1791) H19C(0.2215) H20(0.5068) H21A(0.7022)
 H21B(0.6952) H21C(0.6508) H22A(0.483) H22B(0.5722) H22C(0.6073) H23(0.3481)
 H24A(0.1651) H24B(0.2381) H24C(0.1653) H25A(0.4235) H25B(0.4083) H25C(0.3249)
;
_shelx_res_checksum              85431
_shelx_hkl_checksum              98745