Towards stable and efficient electrolytes for room-temperature rechargeable calcium batteries
Li, Zhenyou; Fuhr, Olaf; Fichtner, Maximilian; Zhao-Karger, Zhirong; Energy & Environmental Science 12 (2019) 3496–; doi:10.1039/C9EE01699F

data_1556887
_publ_section_title
;
 Towards stable and efficient electrolytes for room-temperature
 rechargeable calcium batteries
;
_journal_issue                   12
_journal_name_full               'Energy &amp; Environmental Science'
_journal_page_first              3496
_journal_paper_doi               10.1039/C9EE01699F
_journal_volume                  12
_journal_year                    2019
_chemical_formula_moiety         'C16 H40 Ca O8, 2(C12 H4 B F24 O4)'
_chemical_formula_sum            'C40 H48 B2 Ca F48 O16'
_chemical_formula_weight         1758.48
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-11 deposited with the CCDC.	2019-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5970(6)
_cell_length_b                   19.5970(6)
_cell_length_c                   36.7108(15)
_cell_measurement_reflns_used    44619
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      2.21
_cell_volume                     14098.5(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            49131
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         2.356
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.8838
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE Xred and LANA'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             7024
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6908
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1750P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5297
_reflns_number_total             6908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ee01699f2.cif
_cod_data_source_block           zz2018-1ca
_cod_original_cell_volume        14098.5(10)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1556887
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.510(3)
 0.490(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O4_$1-O4
 2.65 with sigma of 0.02
 O4-C7
 1.43 with sigma of 0.02
 O4-C8
 1.43 with sigma of 0.02
 Ca1-C8
 3.3 with sigma of 0.02
 C8-C8_$1
 1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim O2 \\sim C3 \\sim C2 \\sim O1 \\sim C1: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C8) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.03 and sigma for terminal atoms of 0.04
Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F13) \\sim Ueq: with sigma of 0.06 and
sigma for terminal atoms of 0.12
Uanis(C7) = Uanis(O4) = Uanis(C8)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C15(H15), C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C8(H8A,H8B)
5.c Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              91912
_shelx_hkl_checksum              36338
_olex2_submission_special_instructions 'No special instructions were received'