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_7245043
_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(C25 H22 P), C4 O4 Pd S4, 2(C H2 Cl2), 0.5(C2 H4 Cl2), Cl'
_chemical_formula_sum            'C57 H50 Cl6 O4 P2 Pd S4'
_chemical_formula_weight         1308.25
_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
_audit_creation_date             2022-01-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                81.465(2)
_cell_angle_beta                 75.796(2)
_cell_angle_gamma                81.299(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7497(5)
_cell_length_b                   10.1139(6)
_cell_length_c                   16.8551(10)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      2.51
_cell_volume                     1419.65(14)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78201
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.293
_diffrn_reflns_theta_min         2.419
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       prism
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.234
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         12550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0218P)^2^+0.9945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11514
_reflns_number_total             12550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00489e2.cif
_cod_data_source_block           nad04pd_0m_b
_cod_original_cell_volume        1419.65(15)
_cod_database_code               7245043
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.752
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C3-Cl3 \\sim C3-Cl4
 with sigma of 0.02
3. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) Cl3(0.5) Cl4(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B), C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57)
;
_shelx_res_checksum              48457
_olex2_submission_special_instructions 'No special instructions were received'