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_4130041
_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         'C25 H47 Au Cl N6 P'
_chemical_formula_sum            'C25 H47 Au Cl N6 P'
_chemical_formula_weight         695.07
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5693(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3449(4)
_cell_length_b                   9.8012(2)
_cell_length_c                   17.5758(4)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.079
_cell_measurement_theta_min      2.333
_cell_volume                     2968.28(11)
_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      100.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41480
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.094
_diffrn_reflns_theta_min         3.126
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.124
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.4524.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.875
_refine_diff_density_min         -1.808
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0242
_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^)+8.7073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6228
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13116_si_003.cif
_cod_data_source_block           compound6
_cod_database_code               4130041
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.049) H4B(0.049) H4C(0.049) H5A(0.042) H5B(0.042) H5C(0.042)
 H6(0.033) H7A(0.075) H7B(0.075) H7C(0.075) H8A(0.082) H8B(0.082) H8C(0.082)
 H9(0.03) H10A(0.056) H10B(0.056) H10C(0.056) H11A(0.049) H11B(0.049)
 H11C(0.049) H15A(0.051) H15B(0.051) H15C(0.051) H16A(0.04) H16B(0.04)
 H16C(0.04) H17(0.039) H18A(0.082) H18B(0.082) H18C(0.082) H19A(0.048)
 H19B(0.048) H19C(0.048) H20(0.02) H21A(0.033) H21B(0.033) H21C(0.033)
 H22A(0.035) H22B(0.035) H22C(0.035) H23(0.036) H24A(0.065) H24B(0.065)
 H24C(0.065) H25A(0.059) H25B(0.059) H25C(0.059)
 Fixed X: H4A(0.4886) H4B(0.3969) H4C(0.4316) H5A(0.3091) H5B(0.3163)
 H5C(0.2796) H6(0.6051) H7A(0.5391) H7B(0.5312) H7C(0.6141) H8A(0.6836)
 H8B(0.6429) H8C(0.612) H9(0.4442) H10A(0.4581) H10B(0.4042) H10C(0.3657)
 H11A(0.3168) H11B(0.3266) H11C(0.2856) H15A(0.5139) H15B(0.4344) H15C(0.5142)
 H16A(0.2967) H16B(0.3262) H16C(0.2983) H17(0.6394) H18A(0.6421) H18B(0.7138)
 H18C(0.6466) H19A(0.5949) H19B(0.6784) H19C(0.6024) H20(0.4038) H21A(0.2668)
 H21B(0.2736) H21C(0.3153) H22A(0.4045) H22B(0.3237) H22C(0.328) H23(0.6364)
 H24A(0.7083) H24B(0.7527) H24C(0.6928) H25A(0.6097) H25B(0.7013) H25C(0.6539)
 Fixed Y: H4A(1.1325) H4B(1.1186) H4C(1.1335) H5A(0.9634) H5B(0.8181)
 H5C(0.8287) H6(0.8485) H7A(1.1095) H7B(0.9849) H7C(1.0533) H8A(1.0029)
 H8B(0.9048) H8C(1.0575) H9(0.5177) H10A(0.6182) H10B(0.4852) H10C(0.6337)
 H11A(0.4436) H11B(0.5436) H11C(0.5971) H15A(0.9228) H15B(0.8525) H15C(0.7693)
 H16A(0.7098) H16B(0.8329) H16C(0.8621) H17(0.6937) H18A(0.8642) H18B(0.8208)
 H18C(0.9157) H19A(0.5153) H19B(0.5651) H19C(0.6048) H20(0.6906) H21A(0.6872)
 H21B(0.639) H21C(0.5531) H22A(0.9268) H22B(0.879) H22C(0.9227) H23(0.4131)
 H24A(0.6418) H24B(0.5289) H24C(0.6307) H25A(0.329) H25B(0.3467) H25C(0.4553)
 Fixed Z: H4A(0.4167) H4B(0.4185) H4C(0.3384) H5A(0.4373) H5B(0.4791)
 H5C(0.3915) H6(0.3063) H7A(0.2792) H7B(0.22) H7C(0.2442) H8A(0.3756)
 H8B(0.4318) H8C(0.4168) H9(0.3997) H10A(0.5245) H10B(0.5186) H10C(0.5182)
 H11A(0.3897) H11B(0.3195) H11C(0.3909) H15A(-0.0659) H15B(-0.1009) H15C(-
 0.097) H16A(-0.0007) H16B(-0.0498) H16C(0.0324) H17(0.1037) H18A(-0.0226)
 H18B(0.038) H18C(0.0642) H19A(0.0273) H19B(0.0082) H19C(-0.0477) H20(0.2226)
 H21A(0.1167) H21B(0.2042) H21C(0.1431) H22A(0.2113) H22B(0.2383) H22C(0.1511)
 H23(0.3168) H24A(0.2526) H24B(0.307) H24C(0.3404) H25A(0.1943) H25B(0.216)
 H25C(0.1611)
;
_shelx_res_checksum              29355
_shelx_hkl_checksum              35116