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_7133902
_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         'C25 H28 N2 O2 S2'
_chemical_formula_sum            'C25 H28 N2 O2 S2'
_chemical_formula_weight         452.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-09
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.023(5)
_cell_length_b                   8.7121(14)
_cell_length_c                   17.796(3)
_cell_measurement_reflns_used    1086
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.474
_cell_measurement_theta_min      3.265
_cell_volume                     4809.8(14)
_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      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1415
_diffrn_reflns_av_unetI/netI     0.1364
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27140
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.338
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1487 before and 0.0964 after correction.
The Ratio of minimum to maximum transmission is 0.7534.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1902 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         8467
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0753
_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^)+(0.0574P)^2^+4.0713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                6097
_reflns_number_total             8467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04582c2.cif
_cod_data_source_block           pca21_mer_084
_cod_depositor_comments
'Adding full bibliography for 7133902--7133905.cif.'
_cod_original_cell_volume        4809.7(13)
_cod_database_code               7133902
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.976
_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.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C26(H26), C32(H32), C34(H34), C50(H50), C27(H27), C15(H15), C9(H9)
2.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C31(H31A,H31B,
 H31C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C19(H19A,H19B,H19C), C39(H39A,
 H39B,H39C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C),
 C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C), C3(H3A,H3B,H3C),
  C49(H49A,H49B,H49C)
;
_shelx_res_checksum              84961
_shelx_hkl_checksum              63493
_olex2_submission_special_instructions 'No special instructions were received'