Highly effective capture and subsequent catalytic transformation of low-concentration CO2 by superbasic guanidines
Zhou, Hui; Chen, Wei; Liu, Ji-Hong; Zhang, Wen-Zhen; Lu, Xiao-Bing; Green Chemistry 22 (2020) 7832–7838; doi:10.1039/D0GC03009K

data_7241413
_publ_section_title
;
 Highly effective capture and subsequent catalytic transformation of
 low-concentration CO2 by superbasic guanidines
;
_journal_issue                   22
_journal_name_full               'Green Chemistry'
_journal_page_first              7832
_journal_page_last               7838
_journal_paper_doi               10.1039/D0GC03009K
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety
'2(C H O3), C26 H48 N7, C26 H47 N7, H2 O, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H115 N14 O9'
_chemical_formula_weight         1200.67
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2020-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                63.9960(10)
_cell_angle_beta                 70.8360(10)
_cell_angle_gamma                69.4750(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8442(7)
_cell_length_b                   17.5019(9)
_cell_length_c                   18.6407(9)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.33
_cell_volume                     3450.4(3)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22567
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.352
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1062 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.8115.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         12780
_refine_ls_number_restraints     1981
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1420P)^2^+2.4493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2280
_refine_ls_wR_factor_ref         0.2485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9588
_reflns_number_total             12780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0gc03009k2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7241409--7241413.cif.'
_cod_database_code               7241413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H5-O5
 0.84 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C12 \\sim C6 \\sim C16 \\sim C38 \\sim C9 \\sim C32 \\sim C5 \\sim C4 \\sim C42
\\sim C43 \\sim C31 \\sim C30 \\sim C44 \\sim C50 \\sim C11 \\sim C17 \\sim C39
\\sim C8 \\sim C19 \\sim C24 \\sim C28 \\sim C18 \\sim C34 \\sim C7 \\sim C2
\\sim C59 \\sim C45 \\sim C62 \\sim C13 \\sim C21 \\sim C20 \\sim C27 \\sim C35
\\sim C41 \\sim C1 \\sim C10 \\sim C33 \\sim C3 \\sim C60 \\sim C37 \\sim C46
\\sim C23 \\sim C47 \\sim C22 \\sim C25 \\sim C26 \\sim C29 \\sim C61 \\sim C36
\\sim C15 \\sim C40 \\sim C14 \\sim C49 \\sim C49A \\sim C48 \\sim C54 \\sim
C53 \\sim C52 \\sim C51 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim C54A
\\sim C53A \\sim C52A \\sim C51A \\sim C58A \\sim C55A \\sim C56A \\sim C57A
\\sim O5 \\sim O6 \\sim O4 \\sim O1 \\sim O3 \\sim O2 \\sim O01E \\sim O7 \\sim
O8 \\sim O7A \\sim O8A: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(O7A)=Sof(C54A)=Sof(H54C)=
 Sof(H54D)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(C51A)=Sof(H51C)=Sof(H51D)=Sof(C58A)=Sof(H58C)=Sof(H58D)=Sof(O8A)=Sof(C55A)=
 Sof(H55C)=Sof(H55D)=Sof(C56A)=Sof(H56C)=Sof(H56D)=Sof(C57A)=Sof(H57C)=
 Sof(H57D)=1-FVAR(1)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(O7)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C51)=Sof(H51A)=
 Sof(H51B)=Sof(O8)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C57)=Sof(H57A)=Sof(H57B)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C55)=Sof(H55A)=Sof(H55B)=FVAR(1)
5.a Riding coordinates:
 O5(H5), O01E(H01A,H01B), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C)
5.b Ternary CH refined with riding coordinates:
 C9(H9), C39(H39), C19(H19), C24(H24), C28(H28), C2(H2), C59(H59), C13(H13),
 C35(H35)
5.c Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C53(H53A,H53B), C52(H52A,H52B), C51(H51A,H51B), C58(H58A,
 H58B), C57(H57A,H57B), C56(H56A,H56B), C55(H55A,H55B), C54A(H54C,H54D),
 C53A(H53C,H53D), C52A(H52C,H52D), C51A(H51C,H51D), C58A(H58C,H58D), C55A(H55C,
 H55D), C56A(H56C,H56D), C57A(H57C,H57D)
5.d Aromatic/amide H refined with riding coordinates:
 N12(H12), N7(H7)
5.e Fitted pentagon refined as free rotating group:
 O7(C54,C53,C52,C51), O8(C58,C57,C56,C55), O7A(C54A,C53A,C52A,C51A), C58A(O8A,
 C55A,C56A,C57A)
5.f Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C34(H34A,H34B,H34C), C7(H7A,H7B,H7C),
 C45(H45A,H45B,H45C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C41(H41A,H41B,H41C), C33(H33A,H33B,H33C), C3(H3A,H3B,H3C), C60(H60A,
 H60B,H60C), C37(H37A,H37B,H37C), C46(H46A,H46B,H46C), C23(H23A,H23B,H23C),
 C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C29(H29A,H29B,
 H29C), C61(H61A,H61B,H61C), C36(H36A,H36B,H36C), C15(H15A,H15B,H15C), C40(H40A,
 H40B,H40C), C14(H14A,H14B,H14C), C49(H49A,H49B,H49C), C49A(H49D,H49E,H49F),
 C48(H48A,H48B,H48C)
5.g Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'