Unmasking the constitution and bonding of the proposed lithium nickelate “Li3NiPh3(solv)3”: Revealing the hidden C6H4 ligand
Somerville, Rosie J.; Campos, Jesús; Carmona, Ernesto; Grabowsky, Simon; Malaspina, Lorraine A.; Balcells, David; Hevia, Eva; Nova, Ainara; Pérez-Jiménez, Marina; Borys, Andryj M.; Chemical Science  (2022) –; doi:10.1039/D2SC01244H

data_1566778
_publ_section_title
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 Unmasking the constitution and bonding of the proposed lithium nickelate
 &#x201C;Li3NiPh3(solv)3&#x201D;: Revealing the hidden C6H4 ligand
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01244H
_journal_year                    2022
_chemical_formula_moiety         'C58 H73 Li6 Ni2 O4'
_chemical_formula_sum            'C58 H73 Li6 Ni2 O4'
_chemical_formula_weight         993.22
_chemical_melting_point          ?
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2021-07-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
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_audit_update_record
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2021-12-09 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                101.573(3)
_cell_angle_beta                 103.502(4)
_cell_angle_gamma                101.439(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1760(12)
_cell_length_b                   14.1453(12)
_cell_length_c                   15.9321(15)
_cell_measurement_reflns_used    4764
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.32
_cell_volume                     2733.3(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.1336
_diffrn_reflns_av_unetI/netI     0.1139
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42749
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.511
_diffrn_reflns_theta_min         1.361
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       prism
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         11282
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+2.3160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6349
_reflns_number_total             11282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01244h5.cif
_cod_data_source_block           3_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1566778
_shelx_shelxl_version_number     2014/7
_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. Rigid bond restraints
3. Uiso/Uaniso restraints and constraints
C48 \\sim C47 \\sim O4 \\sim C45 \\sim C46: within 2A with sigma of 0.00001 and
sigma for terminal atoms of 0.00002 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C51(H51A,H51B), C41(H41A,H41B), C43(H43A,
 H43B), C47(H47A,H47B), C49(H49A,H49B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C56(H56), C20(H20), C30(H30), C6(H6), C57(H57), C18(H18), C12(H12),
 C8(H8), C23(H23), C10(H10), C2(H2), C14(H14), C26(H26), C5(H5), C29(H29),
 C16(H16), C22(H22), C21(H21), C11(H11), C9(H9), C27(H27), C17(H17), C32(H32),
 C28(H28), C15(H15), C4(H4), C3(H3), C33(H33), C36(H36), C34(H34), C35(H35),
 C45(H45)
4.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C48(H48A,
 H48B,H48C)
;
_shelx_res_checksum              77202
_shelx_hkl_checksum              51139
_olex2_submission_special_instructions 'No special instructions were received'