On the incompatibility of lithium-O2 battery technology with CO2
Zhang, Shiyu; Nava, Matthew Jordan; Chow, Gary; Lopez, Nazario; Wu, Gang; Britt, R. David; Nocera, Daniel G.; Cummins, Christopher; Chem. Sci.  (2017) –; doi:10.1039/C7SC01230F

data_1546357
_publ_section_title
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 On the incompatibility of lithium-O2 battery technology with CO2
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_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01230F
_journal_year                    2017
_chemical_formula_sum            'C66 H101 K N10 O12'
_chemical_formula_weight         1265.66
_chemical_name_systematic        '[K(Kryptofix-2,2,2)][mBDCA-5t-5H]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-10-28 deposited with the CCDC.
2017-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.616(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.565(3)
_cell_length_b                   20.3058(16)
_cell_length_c                   22.5109(18)
_cell_measurement_reflns_used    9568
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.27
_cell_measurement_theta_min      2.26
_cell_volume                     15074(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_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, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0802
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            247025
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         1.235
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1234 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.8908.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       block
_exptl_crystal_F_000             5456
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN/Ether'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.053
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         22903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0765P)^2^+2.6527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14719
_reflns_number_total             22903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01230f2.cif
_cod_data_source_block           K222_5t_5H
_cod_database_code               1546357
_shelx_estimated_absorpt_t_max   0.7461
_shelx_estimated_absorpt_t_min   0.6646
_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
2.a Secondary CH2 refined with riding coordinates:
 C112(H11A,H11B), C212(H21A,H21B), C311(H31A,H31B), C211(H21C,H21D), C111(H11C,
 H11D), C312(H31C,H31D), C201(H20A,H20B), C202(H20C,H20D), C102(H10A,H10B),
 C101(H10C,H10D), C302(H30A,H30B), C301(H30C,H30D), C8K(H8KA,H8KB), C18K(H18A,
 H18B), C17K(H17A,H17B), C9K(H9KA,H9KB), C12K(H12A,H12B), C15K(H15A,H15B),
 C16K(H16A,H16B), C1K(H1KA,H1KB), C7K(H7KA,H7KB), C2K(H2KA,H2KB), C10K(H10E,
 H10F), C5K(H5KA,H5KB), C13K(H13A,H13B), C6K(H6KA,H6KB), C11K(H11N,H11O),
 C14K(H14A,H14B), C3K(H3KA,H3KB), C4K(H4KA,H4KB)
2.b Aromatic/amide H refined with riding coordinates:
 N101(H101), N102(H102), N202(H202), N201(H201), N301(H301), C109(H109),
 C107(H107), C105(H105), C307(H307), C209(H209), C309(H309), C207(H207),
 C205(H205), C305(H305)
2.c Idealised Me refined as rotating group:
 C315(H31E,H31F,H31G), C115(H11E,H11F,H11G), C314(H31H,H31I,H31J), C316(H31K,
 H31L,H31M), C116(H11H,H11I,H11J), C114(H11K,H11L,H11M), C216(H21E,H21F,H21G),
 C214(H21H,H21I,H21J), C215(H21K,H21L,H21M)
;
_shelx_res_checksum              53941
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'