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_7133905
_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 Ni4 O8 S8, C2 H3 N'
_chemical_formula_sum            'C102 H115 N9 Ni4 O8 S8'
_chemical_formula_weight         2086.34
_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             2024-09-05
_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                89.171(2)
_cell_angle_beta                 84.225(2)
_cell_angle_gamma                76.607(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1288(8)
_cell_length_b                   15.5209(8)
_cell_length_c                   21.5815(12)
_cell_measurement_reflns_used    9638
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.125
_cell_measurement_theta_min      2.317
_cell_volume                     4904.6(5)
_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  0.2189
_diffrn_reflns_av_unetI/netI     0.0620
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            299389
_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         2.318
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1501 before and 0.0906 after correction.
The Ratio of minimum to maximum transmission is 0.7534.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         17932
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0373P)^2^+2.0605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13762
_reflns_number_total             17932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04582c2.cif
_cod_data_source_block           p-1-083_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7133902--7133905.cif.'
_cod_database_code               7133905
_shelx_shelxl_version_number     2019/3
_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
 N9-C101
 1.14 with sigma of 0.02
 C101-N9
 1.137 with sigma of 0.01
 C101-C102
 1.456 with sigma of 0.01
 C102-N9
 2.593 with sigma of 0.02
 N9-C102
 2.59 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N9 \\sim C101 \\sim C102: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C101) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C102) \\sim Ueq: with sigma
of 0.004 and sigma for terminal atoms of 0.008
Uanis(C102) = Uanis(C101) = Uanis(N9)
4. Rigid body (RIGU) restrains
 N9, C101, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C51(H51), C57(H57), C73(H73), C81(H81), C85(H85), C89(H89), C91(H91),
 C99(H99), C26(H26), C58(H58), C17(H17), C34(H34), C72(H72), C19(H19), C38(H38),
  C21(H21)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C22(H22A,H22B,H22C), C43(H43A,H43B,H43C), C47(H47A,H47B,
 H47C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C75(H75A,H75B,H75C), C95(H95A,
 H95B,H95C), C97(H97A,H97B,H97C), C13(H13A,H13B,H13C), C64(H64A,H64B,H64C),
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C36(H36A,H36B,
 H36C), C76(H76A,H76B,H76C), C80(H80A,H80B,H80C), C40(H40A,H40B,H40C), C84(H84A,
 H84B,H84C), C42(H42A,H42B,H42C), C11(H11A,H11B,H11C), C88(H88A,H88B,H88C),
 C44(H44A,H44B,H44C), C90(H90A,H90B,H90C), C23(H23A,H23B,H23C), C92(H92A,H92B,
 H92C), C46(H46A,H46B,H46C), C94(H94A,H94B,H94C), C3(H3A,H3B,H3C), C96(H96A,
 H96B,H96C), C48(H48A,H48B,H48C), C98(H98A,H98B,H98C), C102(H10A,H10B,H10C)
;
_shelx_res_checksum              34458
_shelx_hkl_checksum              20163
_olex2_submission_special_instructions 'No special instructions were received'