From lithium to sodium: Design of heterometallic molecular precursors for the NaMO2 cathode materials
Han, Haixiang; Zhou, Zheng; Carozza, Jesse C.; Lengyel, Jeff; Yao, Yuan; Wei, Zheng; Dikarev, Evgeny V.; Chemical Communications  (2019) –; doi:10.1039/C9CC02836F

data_7123573
_publ_section_title
;
 From lithium to sodium: Design of heterometallic molecular precursors for
 the NaMO2 cathode materials
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02836F
_journal_year                    2019
_chemical_formula_moiety         'C56 H94 Co2 Na2 O20'
_chemical_formula_sum            'C56 H94 Co2 Na2 O20'
_chemical_formula_weight         1251.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                96.319(3)
_cell_angle_beta                 92.385(3)
_cell_angle_gamma                106.847(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9404(11)
_cell_length_b                   13.6413(16)
_cell_length_c                   25.787(3)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      3.02
_cell_volume                     3316.4(7)
_computing_cell_refinement       'SAINT V.8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V.8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            82996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2, Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       rod
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         11654
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0288P)^2^+2.0442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7743
_reflns_number_total             11654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02836f2.cif
_cod_data_source_block           naco
_cod_database_code               7123573
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. 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
2. Shared sites
{C45, C45X}
3. Uiso/Uaniso restraints and constraints
O19 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim O19X \\sim C49X \\sim C50X
\\sim C51X \\sim C52X \\sim O20 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
O20X \\sim C53X \\sim C54X \\sim C55X \\sim C56X: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C45X \\sim C46X \\sim C47X \\sim C48X:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C45) = Uanis(C45X)
4. Rigid body (RIGU) restrains
 O19, C49, C50, C51, C52, O19X, C49X, C50X, C51X, C52X, O20, C53, C54, C55,
 C56, O20X, C53X, C54X, C55X, C56X, C45, C46, C47, C48, C45X, C46X, C47X, C48X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O19, C49, C50, C51, C52} sigma for 1-2: 0.02, 1-3: 0.04
as
{O19X, C49X, C50X, C51X, C52X}
{O20, C53, C54, C55, C56} sigma for 1-2: 0.02, 1-3: 0.04
as
{O20X, C53X, C54X, C55X, C56X}
{C45, C46, C47, C48} sigma for 1-2: 0.02, 1-3: 0.04
as
{C45X, C46X, C47X, C48X}
6. Others
 Sof(O19X)=Sof(C49X)=Sof(H49C)=Sof(H49D)=Sof(C50X)=Sof(H50C)=Sof(H50D)=
 Sof(C51X)=Sof(H51C)=Sof(H51D)=Sof(C52X)=Sof(H52C)=Sof(H52D)=1-FVAR(1)
 Sof(O19)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=
 Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(1)
 Sof(O20X)=Sof(C53X)=Sof(H53C)=Sof(H53D)=Sof(C54X)=Sof(H54C)=Sof(H54D)=
 Sof(C55X)=Sof(H55C)=Sof(H55D)=Sof(C56X)=Sof(H56C)=Sof(H56D)=1-FVAR(2)
 Sof(O20)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C55)=
 Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=FVAR(2)
 Sof(C46X)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47X)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C48X)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(3)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(3)
 Fixed Sof: C45X(0)
7.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C49X(H49C,
 H49D), C50X(H50C,H50D), C51X(H51C,H51D), C52X(H52C,H52D), C53(H53A,H53B),
 C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C53X(H53C,H53D), C54X(H54C,
 H54D), C55X(H55C,H55D), C56X(H56C,H56D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C19(H19), C27(H27), C35(H35), C43(H43)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C46X(H46D,H46E,H46F), C47X(H47D,H47E,H47F),
 C48X(H48D,H48E,H48F)
;
_shelx_res_checksum              38731
_olex2_submission_special_instructions 'No special instructions were received'