Diamidocarbene-derived palladium and nickel-sulfur clusters.
Lee, Minji; Noh, Hyunju; Kim, Youngsuk; Chemical communications (Cambridge, England) 60 (2024) 13867–13870; doi:10.1039/d4cc04582c

data_7133903
_publ_section_title
;
 Diamidocarbene-derived palladium and nickel-sulfur clusters.
;
_journal_issue                   94
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13867
_journal_page_last               13870
_journal_paper_doi               10.1039/d4cc04582c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C100 H112 N8 Ni3 O8 S8, 0.848(C4 H10 O), 1.681(C2 H3 N)'
_chemical_formula_sum            'C106.75 H125.53 N9.68 Ni3 O8.85 S8'
_chemical_formula_weight         2118.48
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-09 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                89.342(4)
_cell_angle_beta                 89.718(4)
_cell_angle_gamma                66.280(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1896(15)
_cell_length_b                   16.1897(18)
_cell_length_c                   25.073(2)
_cell_measurement_reflns_used    9481
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.56
_cell_volume                     5273.0(9)
_computing_cell_refinement       'Bruker APEX4 software'
_computing_data_collection       'Bruker APEX4 software'
_computing_data_reduction        'Bruker APEX4 software'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1328
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            217573
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.188
_diffrn_reflns_theta_max         25.188
_diffrn_reflns_theta_min         1.816
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.6918
_exptl_absorpt_correction_T_min  0.5288
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             2233
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         18939
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0887
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1587P)^2^+40.8718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2396
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15247
_reflns_number_total             18939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04582c2.cif
_cod_data_source_block           1007re
_cod_depositor_comments
'Adding full bibliography for 7133902--7133905.cif.'
_cod_original_cell_volume        5272.9(10)
_cod_database_code               7133903
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7945(13)
 0.2055(13)
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
 O311-C310 = O311-C312
 1.45 with sigma of 0.02
 C310-C309 = C312-C313
 1.54 with sigma of 0.02
 C310-C312
 2.4 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(N314) \\sim Ueq, Uanis(C315) \\sim Ueq, Uanis(C316) \\sim Ueq,
Uanis(O311) \\sim Ueq, Uanis(C310) \\sim Ueq, Uanis(C309) \\sim Ueq,
Uanis(C312) \\sim Ueq, Uanis(C313) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C302) \\sim Ueq, Uanis(C301) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 N314, C315, C316, O311, C310, C309, C312, C313
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O303)=Sof(C304)=Sof(H30D)=Sof(H30E)=Sof(C305)=Sof(H30F)=Sof(H30G)=
 Sof(H30H)=Sof(C302)=Sof(H30I)=Sof(H30J)=Sof(C301)=Sof(H30K)=Sof(H30L)=
 Sof(H30M)=FVAR(1)
 Sof(O311)=Sof(C310)=Sof(H31A)=Sof(H31B)=Sof(C309)=Sof(H30N)=Sof(H30O)=
 Sof(H30P)=Sof(C312)=Sof(H31C)=Sof(H31D)=Sof(C313)=Sof(H31E)=Sof(H31F)=
 Sof(H31G)=1-FVAR(2)
 Sof(N314)=Sof(C315)=Sof(C316)=Sof(H31H)=Sof(H31I)=Sof(H31J)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C304(H30D,H30E), C302(H30I,H30J), C310(H31A,H31B), C312(H31C,H31D)
7.b Me refined with riding coordinates:
 C316(H31H,H31I,H31J), C309(H30N,H30O,H30P), C313(H31E,H31F,H31G)
7.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C24(H24), C38(H38), C42(H42), C70(H70), C74(H74), C88(H88),
 C92(H92), C59(H59), C61(H61), C17(H17), C35(H35), C21(H21), C43(H43), C93(H93),
  C95(H95)
7.d Fitted hexagon refined as free rotating group:
 C57(C29,C59,C15,C61,C31), C33(C67,C17,C69,C35,C71), C41(C83,C21,C85,C43,C87),
 C91(C23,C93,C47,C95,C3)
7.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,
 H50B,H50C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C78(H78A,H78B,H78C),
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C96(H96A,H96B,H96C), C98(H98A,H98B,
 H98C), C100(H10D,H10E,H10F), C110(H11A,H11B,H11C), C112(H11D,H11E,H11F),
 C63(H63A,H63B,H63C), C2(H2A,H2B,H2C), C65(H65A,H65B,H65C), C9(H9A,H9B,H9C),
 C73(H73A,H73B,H73C), C37(H37A,H37B,H37C), C79(H79A,H79B,H79C), C5(H5A,H5B,H5C),
  C11(H11G,H11H,H11I), C89(H89A,H89B,H89C), C45(H45A,H45B,H45C), C97(H97A,H97B,
 H97C), C49(H49A,H49B,H49C), C99(H99A,H99B,H99C), C305(H30F,H30G,H30H),
 C301(H30K,H30L,H30M), C306(H30Q,H30R,H30S)
;
_shelx_res_checksum              74417
_shelx_hkl_checksum              44481
_olex2_submission_special_instructions 'No special instructions were received'