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_7133904
_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 O8 Pd4 S8, C2 H3 N'
_chemical_formula_sum            'C102 H115 N9 O8 Pd4 S8'
_chemical_formula_weight         2277.10
_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             2024-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                89.1590(10)
_cell_angle_beta                 83.5970(10)
_cell_angle_gamma                76.3130(10)
_cell_formula_units_Z            2
_cell_length_a                   15.1195(5)
_cell_length_b                   15.5620(5)
_cell_length_c                   21.9749(7)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.543
_cell_measurement_theta_min      2.201
_cell_volume                     4991.9(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_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  0.0845
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            288654
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.415
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.937
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1253 before and 0.0772 after correction.
The Ratio of minimum to maximum transmission is 0.9117.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             2332
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1240
_refine_ls_number_reflns         18271
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+6.1848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15901
_reflns_number_total             18271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04582c2.cif
_cod_data_source_block           p-1-083
_cod_depositor_comments
'Adding full bibliography for 7133902--7133905.cif.'
_cod_database_code               7133904
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N301-C302
 1.14 with sigma of 0.02
 C302-C303
 1.456 with sigma of 0.01
 C302-N301
 1.137 with sigma of 0.01
 C303-N301
 2.593 with sigma of 0.02
 N301-C303
 2.59 with sigma of 0.04
 C302-C303 \\sim C101-C1A
 with sigma of 0.02
 N301-C303 \\sim N9-C1A
 with sigma of 0.04
 N301-C302 \\sim N9-C101
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N301 \\sim C302 \\sim C303: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C1A) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C302) \\sim Ueq, Uanis(N301) \\sim Ueq, Uanis(C303) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N301, C302, C303
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, N9, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C302, N301, C303
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N9)=Sof(C101)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(N301)=Sof(C302)=Sof(C303)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
6.a Me refined with riding coordinates:
 C303(H30A,H30B,H30C), C1A(H1AA,H1AB,H1AC)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C14(H14), C18(H18), C38(H38), C50(H50), C52(H52), C70(H70),
 C96(H96), C15(H15), C31(H31), C85(H85), C87(H87), C89(H89), C93(H93), C47(H47)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C40(H40A,H40B,H40C), C68(H68A,H68B,
 H68C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C88(H88A,H88B,H88C), C25(H25A,
 H25B,H25C), C53(H53A,H53B,H53C), C7(H7A,H7B,H7C), C57(H57A,H57B,H57C),
 C29(H29A,H29B,H29C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C33(H33A,H33B,
 H33C), C67(H67A,H67B,H67C), C35(H35A,H35B,H35C), C71(H71A,H71B,H71C), C9(H9A,
 H9B,H9C), C73(H73A,H73B,H73C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C81(H81A,H81B,H81C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C91(H91A,H91B,H91C), C95(H95A,H95B,H95C), C3(H3A,
 H3B,H3C), C49(H49A,H49B,H49C), C99(H99A,H99B,H99C)
;
_shelx_res_checksum              82965
_shelx_hkl_checksum              19077
_olex2_submission_special_instructions 'No special instructions were received'