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_4130040
_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 N6 P'
_chemical_formula_sum            'C25 H47 N6 P'
_chemical_formula_weight         462.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 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                 109.3590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2900(4)
_cell_length_b                   11.5237(3)
_cell_length_c                   13.3929(3)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.238
_cell_measurement_theta_min      2.894
_cell_volume                     2663.20(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      100.03
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16952
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.245
_diffrn_reflns_theta_min         3.521
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0907 before and 0.0315 after correction.
The Ratio of minimum to maximum transmission is 0.8770.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0550P)^2^+0.6379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                6246
_reflns_number_total             6346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13116_si_001.cif
_cod_data_source_block           compound5
_cod_database_code               4130040
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.032) H4B(0.032) H4C(0.032) H5A(0.033) H5B(0.033) H5C(0.033)
 H6(0.022) H7A(0.036) H7B(0.036) H7C(0.036) H8A(0.039) H8B(0.039) H8C(0.039)
 H9(0.02) H10A(0.036) H10B(0.036) H10C(0.036) H11A(0.036) H11B(0.036)
 H11C(0.036) H15A(0.037) H15B(0.037) H15C(0.037) H16A(0.038) H16B(0.038)
 H16C(0.038) H17(0.024) H18A(0.037) H18B(0.037) H18C(0.037) H19A(0.041)
 H19B(0.041) H19C(0.041) H20(0.022) H21A(0.049) H21B(0.049) H21C(0.049)
 H22A(0.036) H22B(0.036) H22C(0.036) H23(0.023) H24A(0.039) H24B(0.039)
 H24C(0.039) H25A(0.046) H25B(0.046) H25C(0.046)
 Fixed X: H4A(-0.0265) H4B(-0.0274) H4C(0.0291) H5A(-0.2012) H5B(-0.1102) H5C(-
 0.1469) H6(-0.0857) H7A(-0.0924) H7B(-0.1656) H7C(-0.0976) H8A(0.0328)
 H8B(0.0434) H8C(0.0397) H9(-0.2594) H10A(-0.3369) H10B(-0.319) H10C(-0.2747)
 H11A(-0.1518) H11B(-0.2196) H11C(-0.1524) H15A(-0.535) H15B(-0.5941) H15C(-
 0.5854) H16A(-0.544) H16B(-0.5685) H16C(-0.4896) H17(-0.468) H18A(-0.4021)
 H18B(-0.4335) H18C(-0.4924) H19A(-0.3449) H19B(-0.3477) H19C(-0.3072) H20(-
 0.3449) H21A(-0.322) H21B(-0.341) H21C(-0.4059) H22A(-0.4977) H22B(-0.4321)
 H22C(-0.4679) H23(-0.1752) H24A(-0.2976) H24B(-0.2272) H24C(-0.2115) H25A(-
 0.2708) H25B(-0.2728) H25C(-0.3367)
 Fixed Y: H4A(-0.43) H4B(-0.5476) H4C(-0.5353) H5A(-0.3581) H5B(-0.336) H5C(-
 0.3501) H6(-0.8513) H7A(-0.7109) H7B(-0.7732) H7C(-0.8495) H8A(-0.8642) H8B(-
 0.7871) H8C(-0.7261) H9(-0.6382) H10A(-0.482) H10B(-0.491) H10C(-0.397) H11A(-
 0.5987) H11B(-0.5148) H11C(-0.4651) H15A(-0.5385) H15B(-0.5588) H15C(-0.6549)
 H16A(-0.6453) H16B(-0.5492) H16C(-0.535) H17(-0.6848) H18A(-0.9069) H18B(-
 0.8634) H18C(-0.8802) H19A(-0.6027) H19B(-0.6877) H19C(-0.7294) H20(-0.8234)
 H21A(-0.6329) H21B(-0.7186) H21C(-0.6308) H22A(-0.8018) H22B(-0.8865) H22C(-
 0.9087) H23(-1.0228) H24A(-1.0333) H24B(-1.1229) H24C(-0.9929) H25A(-1.0477)
 H25B(-1.1545) H25C(-1.0544)
 Fixed Z: H4A(-0.4116) H4B(-0.4755) H4C(-0.3558) H5A(-0.3881) H5B(-0.3594)
 H5C(-0.267) H6(-0.3755) H7A(-0.553) H7B(-0.5362) H7C(-0.5532) H8A(-0.3984)
 H8B(-0.2952) H8C(-0.4042) H9(-0.2393) H10A(-0.2601) H10B(-0.369) H10C(-0.282)
 H11A(-0.0964) H11B(-0.0892) H11C(-0.129) H15A(-0.5435) H15B(-0.4799) H15C(-
 0.5614) H16A(-0.2158) H16B(-0.3071) H16C(-0.2098) H17(-0.5972) H18A(-0.5326)
 H18B(-0.6528) H18C(-0.5884) H19A(-0.5236) H19B(-0.6194) H19C(-0.4997) H20(-
 0.1565) H21A(-0.0892) H21B(-0.007) H21C(-0.0762) H22A(-0.1478) H22B(-0.0754)
 H22C(-0.2002) H23(-0.2177) H24A(-0.4159) H24B(-0.3744) H24C(-0.4042) H25A(-
 0.1377) H25B(-0.2149) H25C(-0.2514)
;
_shelx_res_checksum              24430
_shelx_hkl_checksum              72882