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_4130039
_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         'C26 H47 N6 O2 P'
_chemical_formula_sum            'C26 H47 N6 O2 P'
_chemical_formula_weight         506.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8097(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1689(2)
_cell_length_b                   9.47360(10)
_cell_length_c                   20.5469(3)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.476
_cell_measurement_theta_min      2.188
_cell_volume                     2879.19(6)
_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(2)
_diffrn_measured_fraction_theta_full 0.996
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51014
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.515
_diffrn_reflns_theta_min         2.859
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0897 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.9420.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.049
_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         8759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0515P)^2^+1.0420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7555
_reflns_number_total             8759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13116_si_002.cif
_cod_data_source_block           compound5a
_cod_database_code               4130039
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.035) H5B(0.035) H5C(0.035) H6A(0.035) H6B(0.035) H6C(0.035)
 H7(0.021) H8A(0.039) H8B(0.039) H8C(0.039) H9A(0.038) H9B(0.038) H9C(0.038)
 H10(0.021) H11A(0.042) H11B(0.042) H11C(0.042) H12A(0.039) H12B(0.039)
 H12C(0.039) H16A(0.031) H16B(0.031) H16C(0.031) H17A(0.046) H17B(0.046)
 H17C(0.046) H18(0.019) H19A(0.03) H19B(0.03) H19C(0.03) H20A(0.036)
 H20B(0.036) H20C(0.036) H21(0.024) H22A(0.044) H22B(0.044) H22C(0.044)
 H23A(0.049) H23B(0.049) H23C(0.049) H24(0.019) H25A(0.033) H25B(0.033)
 H25C(0.033) H26A(0.032) H26B(0.032) H26C(0.032)
 Fixed X: H5A(0.2523) H5B(0.2494) H5C(0.1573) H6A(0.3194) H6B(0.3225)
 H6C(0.3898) H7(0.0624) H8A(0.0673) H8B(0.1676) H8C(0.1379) H9A(-0.0121) H9B(-
 0.0413) H9C(0.0295) H10(0.2402) H11A(0.3934) H11B(0.3789) H11C(0.3913)
 H12A(0.2434) H12B(0.2273) H12C(0.1529) H16A(0.3907) H16B(0.4685) H16C(0.3709)
 H17A(0.5172) H17B(0.5419) H17C(0.5511) H18(0.1567) H19A(0.1696) H19B(0.1252)
 H19C(0.2288) H20A(0.2761) H20B(0.1726) H20C(0.2459) H21(0.3266) H22A(0.3945)
 H22B(0.3338) H22C(0.4414) H23A(0.5171) H23B(0.4556) H23C(0.4643) H24(0.0932)
 H25A(0.0929) H25B(-0.0052) H25C(0.0168) H26A(-0.0274) H26B(-0.0506) H26C(0.021)
 Fixed Y: H5A(0.5191) H5B(0.6645) H5C(0.5842) H6A(0.983) H6B(0.8575)
 H6C(0.8562) H7(0.542) H8A(0.326) H8B(0.3677) H8C(0.3844) H9A(0.6817)
 H9B(0.5204) H9C(0.5912) H10(0.9373) H11A(0.8836) H11B(1.0464) H11C(1.0001)
 H12A(1.1105) H12B(1.164) H12C(1.0679) H16A(0.1511) H16B(0.1123) H16C(0.0407)
 H17A(0.2604) H17B(0.211) H17C(0.3737) H18(0.3255) H19A(0.0934) H19B(0.096)
 H19C(0.0514) H20A(0.2486) H20B(0.2944) H20C(0.4072) H21(0.5684) H22A(0.488)
 H22B(0.3649) H22C(0.3608) H23A(0.5443) H23B(0.6467) H23C(0.6729) H24(0.5463)
 H25A(0.7963) H25B(0.7305) H25C(0.8051) H26A(0.5843) H26B(0.5042) H26C(0.4377)
 Fixed Z: H5A(0.139) H5B(0.0989) H5C(0.1013) H6A(0.191) H6B(0.1394)
 H6C(0.2114) H7(0.2646) H8A(0.2136) H8B(0.2519) H8C(0.1726) H9A(0.1764)
 H9B(0.1621) H9C(0.1246) H10(0.3601) H11A(0.3608) H11B(0.3764) H11C(0.3041)
 H12A(0.2474) H12B(0.3177) H12C(0.2705) H16A(0.5655) H16B(0.5271) H16C(0.505)
 H17A(0.3842) H17B(0.4606) H17C(0.4421) H18(0.4666) H19A(0.4293) H19B(0.4931)
 H19C(0.5013) H20A(0.5889) H20B(0.5804) H20C(0.5684) H21(0.3308) H22A(0.2467)
 H22B(0.2673) H22C(0.2929) H23A(0.3774) H23B(0.4107) H23C(0.3354) H24(0.4796)
 H25A(0.4895) H25B(0.4863) H25C(0.4219) H26A(0.3528) H26B(0.4155) H26C(0.3775)
;
_shelx_res_checksum              56821
_shelx_hkl_checksum              99848