Bulky countercation effects on the crystal packing of anionic dithiooxalato-containing Ni(II), Pd(II) and Pt(II) complexes: spectroscopic-redox correlations
Julve, Miguel; El Alouani Dahmouni, Nadia; Switlicka, Anna; Machura, B.; Moliner, Fernando Nicolás; Rabelo, Renato; Ruiz-Garcia, Rafael; Stiriba, Salah-Eddine; Cano, Joan; CrystEngComm  (2022) –; doi:10.1039/D2CE00489E

data_7245047
_publ_section_title
;
 Bulky countercation effects on the crystal packing of anionic
 dithiooxalato-containing Ni(II), Pd(II) and Pt(II) complexes:
 spectroscopic-redox correlations
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00489E
_journal_year                    2022
_chemical_formula_moiety         '2(C24 H20 As), C4 Ni O4 S4, C3 H6 O'
_chemical_formula_sum            'C55 H46 As2 Ni O5 S4'
_chemical_formula_weight         1123.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-28 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.4267(5)
_cell_length_b                   52.731(2)
_cell_length_c                   13.8477(6)
_cell_measurement_reflns_used    327123
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.52
_cell_volume                     7484.2(6)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      119.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            327123
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.294
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       brick
_exptl_crystal_F_000             3444
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.114
_exptl_transmission_factor_max   0.811
_exptl_transmission_factor_min   0.499
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00018(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1820
_refine_ls_number_reflns         37087
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0234P)^2^+7.9425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0694
_reflns_Friedel_coverage         0.979
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                35674
_reflns_number_total             37087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00489e2.cif
_cod_data_source_block           nea005as_0m_a
_cod_database_code               7245047
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.499
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1(10)
 0(10) 0.10(13) 0.15(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C137) \\sim Ueq, Uanis(C138) \\sim Ueq, Uanis(C140) \\sim Ueq,
Uanis(C141) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C31(H31),
 C30(H30), C32(H32), C33(H33), C36(H36), C35(H35), C39(H39), C38(H38), C37(H37),
  C41(H41), C42(H42), C44(H44), C43(H43), C45(H45), C47(H47), C49(H49),
 C48(H48), C50(H50), C51(H51), C54(H54), C53(H53), C55(H55), C57(H57), C56(H56),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93),
  C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C107(H107), C108(H108), C109(H109),
 C110(H110), C111(H111), C113(H113), C114(H114), C115(H115), C116(H116),
 C117(H117), C119(H119), C120(H120), C121(H121), C122(H122), C123(H123),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C131(H131),
 C132(H132), C133(H133), C134(H134), C135(H135), C137(H137), C138(H138),
 C139(H139), C140(H140), C141(H141), C143(H143), C144(H144), C145(H145),
 C146(H146), C147(H147), C149(H149), C150(H150), C151(H151), C152(H152),
 C153(H153), C155(H155), C156(H156), C157(H157), C158(H158), C159(H159),
 C161(H161), C162(H162), C163(H163), C164(H164), C165(H165)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              61076
_olex2_submission_special_instructions 'No special instructions were received'