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_7061001
_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_formula_moiety         'C40 H52 O4 P2 S4 Zn'
_chemical_formula_sum            'C40 H52 O4 P2 S4 Zn'
_chemical_formula_weight         852.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-08-12
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2021-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.394(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.0546(5)
_cell_length_b                   13.3289(3)
_cell_length_c                   30.1770(7)
_cell_measurement_reflns_used    4966
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      27.9830
_cell_measurement_theta_min      1.9350
_cell_volume                     8466.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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     40.00 110.00   1.00  140.00    --   26.84 178.00 -60.00   70
  2  \w     70.00 116.00   1.00  140.00    --   26.84 178.00 150.00   46
  3  \w    -44.00  56.00   1.00  140.00    --   26.84 -19.00 -30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0097401000
_diffrn_orient_matrix_UB_12      0.0472410000
_diffrn_orient_matrix_UB_13      0.0085582000
_diffrn_orient_matrix_UB_21      0.0312505000
_diffrn_orient_matrix_UB_22      -0.0188677000
_diffrn_orient_matrix_UB_23      0.0034725000
_diffrn_orient_matrix_UB_31      0.0080126000
_diffrn_orient_matrix_UB_32      0.0158176000
_diffrn_orient_matrix_UB_33      -0.0215978000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0979
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            13538
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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            'metallic light blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.112
_refine_diff_density_max         2.101
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.2016
_reflns_number_gt                6427
_reflns_number_total             9100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj03165a2.cif
_cod_data_source_block           zn_4t_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7061001--7061002.cif.'
_cod_database_code               7061001
_chemical_oxdiff_formula         'C320 H416 O32 P16 S32 Zn8'
_reflns_odcompleteness_completeness 98.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C16(H16), C35(H35), C15(H15), C13(H13), C36(H36), C32(H32), C33(H33), C2(H2),
 C3(H3), C22(H22), C12(H12), C6(H6), C23(H23), C25(H25), C26(H26), C5(H5)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C38(H38A,H38B,H38C), C8(H8A,H8B,H8C), C28(H28A,H28B,
 H28C), C40(H40A,H40B,H40C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C29(H29A,
 H29B,H29C)
;
_olex2_date_sample_data_collection 2021-03-01
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 11.705
_oxdiff_exptl_absorpt_empirical_full_min 0.441