Coordination versus spodium bonds in dinuclear Zn(ii) and Cd(ii) complexes with a dithiophosphate ligand
Kumar, Pretam; Frontera, Antonio; Pandey, Sushil K.; New Journal of Chemistry 45 (2021) 19402–19415; doi:10.1039/D1NJ03165A

data_7061002
_publ_section_title
;
 Coordination versus spodium bonds in dinuclear Zn(ii) and Cd(ii)
 complexes with a dithiophosphate ligand
;
_journal_issue                   41
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19402
_journal_page_last               19415
_journal_paper_doi               10.1039/D1NJ03165A
_journal_volume                  45
_journal_year                    2021
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C80 H104 Cd2 O8 P4 S8'
_chemical_formula_sum            'C80 H104 Cd2 O8 P4 S8'
_chemical_formula_weight         1798.79
_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     iterative
_audit_creation_date             2021-09-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-16 deposited with the CCDC.	2021-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                70.284(18)
_cell_angle_beta                 88.794(17)
_cell_angle_gamma                62.94(3)
_cell_formula_units_Z            1
_cell_length_a                   12.083(3)
_cell_length_b                   13.084(3)
_cell_length_c                   16.602(3)
_cell_measurement_reflns_used    2568
_cell_measurement_temperature    150.01(15)
_cell_measurement_theta_max      27.8510
_cell_measurement_theta_min      2.1070
_cell_volume                     2172.7(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -13.00 107.00   1.00   10.91    --   26.84  77.00   0.00  120
  2  \w    -14.00 106.00   1.00   10.91    --   26.84  77.00-120.00  120
  3  \w    -13.00 106.00   1.00   10.91    --   26.84  77.00 120.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1546
_diffrn_reflns_av_unetI/netI     0.1810
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11522
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.857
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.164
_refine_diff_density_max         3.462
_refine_diff_density_min         -3.365
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1708
_refine_ls_R_factor_gt           0.1284
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2987
_refine_ls_wR_factor_ref         0.3939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4876
_reflns_number_total             8789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03165a2.cif
_cod_data_source_block           scs
_cod_depositor_comments
'Adding full bibliography for 7061001--7061002.cif.'
_cod_original_cell_volume        2172.8(10)
_cod_database_code               7061002
_shelx_shelxl_version_number     2017/1
_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:
 C32(H32), C15(H15), C16(H16), C35(H35), C33(H33), C23(H23), C22(H22),
 C36(H36), C25(H25), C12(H12), C13(H13), C6(H6), C5(H5), C26(H26), C3(H3),
 C2(H2)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C39(H39A,H39B,
 H39C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C19(H19A,
 H19B,H19C), C28(H28A,H28B,H28C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C),
 C29(H29A,H29B,H29C)
;
_shelx_res_checksum              75317
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;