Carboxylic acid-tuned nickel(ii) clusters: syntheses, structures, solution behaviours and magnetic properties.
Su, Yan-Min; Ji, Bao-Qian; Shao, Feng; Zhang, Shan-Shan; Jagodič, Marko; Jagličić, Zvonko; Gao, Zhi-Yong; Dou, Jian-Min; Sun, Di; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4355–4362; doi:10.1039/d1dt00165e

data_7706688
_publ_section_title
;
 Carboxylic acid-tuned nickel(ii) clusters: syntheses, structures,
 solution behaviours and magnetic properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4355
_journal_page_last               4362
_journal_paper_doi               10.1039/d1dt00165e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C61 H68 N10 Ni5 O19 S6, C H4 O'
_chemical_formula_sum            'C62 H72 N10 Ni5 O20 S6'
_chemical_formula_weight         1763.20
_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     dual
_audit_creation_date             2020-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2020-09-01 deposited with the CCDC.	2021-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                106.518(6)
_cell_angle_beta                 95.516(6)
_cell_angle_gamma                96.119(6)
_cell_formula_units_Z            2
_cell_length_a                   13.897(9)
_cell_length_b                   14.250(9)
_cell_length_c                   21.731(13)
_cell_measurement_reflns_used    2874
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.520
_cell_measurement_theta_min      2.264
_cell_volume                     4066(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1548
_diffrn_reflns_av_unetI/netI     0.2032
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54058
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.672
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.948
_platon_squeeze_details          TITL
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         16589
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0824P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6425
_reflns_number_total             16589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00165e2.cif
_cod_data_source_block           Ni5a
_cod_depositor_comments
'Adding full bibliography for 7706687--7706689.cif.'
_cod_database_code               7706688
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.948
_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
2. Shared sites
{S9, C3AA}
{C9, S2}
{C2AA, S4}
{S1, C4AA}
{C3, S6}
{S3, C5AA}
{C7, S8}
{S7, C6AA}
{S5, C5}
{C0AA, S10}
{S11, C8AA}
{C11, S12}
3. Restrained distances
 O16-H16
 0.85 with sigma of 0.01
 O20-H20
 0.85 with sigma of 0.01
 O15-H15B
 0.9 with sigma of 0.01
 Ni4-H16
 2.547289 with sigma of 0.02
 C60-H20
 1.974458 with sigma of 0.02
 Ni5-H20
 2.70472 with sigma of 0.02
 C61-H16
 1.882298 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O20 \\sim C60: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C9) = Uanis(S2)
Uanis(S1) = Uanis(C4AA)
Uanis(S11) = Uanis(C8AA)
Uanis(S3) = Uanis(C5AA)
Uanis(C2AA) = Uanis(S1)
Uanis(C2AA) = Uanis(S4)
Uanis(S7) = Uanis(C6AA)
Uanis(C3) = Uanis(S3)
Uanis(C3) = Uanis(S6)
Uanis(S11) = Uanis(C11)
Uanis(C11) = Uanis(S12)
Uanis(S9) = Uanis(C9)
Uanis(S9) = Uanis(C3AA)
Uanis(C7) = Uanis(S8)
Uanis(C7) = Uanis(S7)
Uanis(C0AA) = Uanis(S10)
Uanis(S5) = Uanis(C5)
Uanis(S5) = Uanis(C0AA)
5. Others
 Sof(S2)=Sof(C3AA)=Sof(H3AA)=Sof(H25A)=Sof(H26A)=1-FVAR(1)
 Sof(S9)=Sof(C9)=Sof(H9A)=Sof(H25)=Sof(H26)=FVAR(1)
 Sof(S4)=Sof(C4AA)=Sof(H4AA)=Sof(H6B)=Sof(H8B)=1-FVAR(2)
 Sof(S1)=Sof(C2AA)=Sof(H2AA)=Sof(H6A)=Sof(H8A)=FVAR(2)
 Sof(S6)=Sof(C5AA)=Sof(H5AA)=Sof(H13A)=Sof(H14A)=1-FVAR(3)
 Sof(S3)=Sof(C3)=Sof(H3)=Sof(H13)=Sof(H14)=FVAR(3)
 Sof(S8)=Sof(C6AA)=Sof(H6AA)=Sof(H17A)=Sof(H18A)=1-FVAR(4)
 Sof(S7)=Sof(C7)=Sof(H7)=Sof(H17)=Sof(H18)=FVAR(4)
 Sof(S10)=Sof(C5)=Sof(H5)=Sof(H21A)=Sof(H22A)=1-FVAR(5)
 Sof(S5)=Sof(C0AA)=Sof(H0AA)=Sof(H21)=Sof(H22)=FVAR(5)
 Sof(S12)=Sof(C8AA)=Sof(H8AA)=Sof(H29A)=Sof(H30A)=1-FVAR(6)
 Sof(S11)=Sof(C11)=Sof(H11)=Sof(H29)=Sof(H30)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C41(H41), C42(H42), C53(H53), C54(H54)
6.b Aromatic/amide H refined with riding coordinates:
 N9(H9), C2AA(H2AA), C3(H3), C3AA(H3AA), C4AA(H4AA), C0AA(H0AA), C5AA(H5AA),
 C6(H6A), C6(H6B), C6AA(H6AA), C7(H7), C5(H5), C8(H8A), C8(H8B), C8AA(H8AA),
 C9(H9A), C11(H11), C13(H13), C13(H13A), C14(H14), C14(H14A), C17(H17),
 C17(H17A), C18(H18), C18(H18A), C21(H21), C21(H21A), C22(H22), C22(H22A),
 C25(H25), C25(H25A), C26(H26), C26(H26A), C29(H29), C29(H29A), C30(H30),
 C30(H30A), C33(H33), C38(H38), C45(H45), C50(H50), C57(H57)
6.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C52(H52A,
 H52B,H52C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
6.d Idealised tetrahedral OH refined as rotating group:
 O19(H19)
;
_olex2_submission_special_instructions 'No special instructions were received'