Synthesis, structure and the Hirshfeld surface analysis of three novel metal-tiron coordination complexes
Tiwari, Ranjay K.; Shruti, Ipsha; Behera, J. N.; RSC Advances 11 (2021) 10767–10776; doi:10.1039/D1RA00207D

data_7242406
_publ_section_title
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 Synthesis, structure and the Hirshfeld surface analysis of three novel
 metal-tiron coordination complexes
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              10767
_journal_page_last               10776
_journal_paper_doi               10.1039/D1RA00207D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C52 H50 Cd2 N8 O20 S4, 0.5(O2)'
_chemical_formula_sum            'C52 H50 Cd2 N8 O21 S4'
_chemical_formula_weight         1474.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-01
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.04.02 svn.r1fbe7b6f for OlexSys, GUI svn.r6076)
;
_audit_update_record
;
2021-01-10 deposited with the CCDC.	2021-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.009(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3724(2)
_cell_length_b                   33.4103(9)
_cell_length_c                   11.7744(3)
_cell_measurement_reflns_used    5130
_cell_measurement_temperature    296.15(2)
_cell_measurement_theta_max      21.24
_cell_measurement_theta_min      2.44
_cell_volume                     2813.94(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0800
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            43935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.884
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0670 before and 0.0597 after correction. The Ratio of minimum to maximum transmission is 0.9236. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_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^+3.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4271
_reflns_number_total             5747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00207d2.cif
_cod_data_source_block           1
_cod_database_code               7242406
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All S(H,H,H,H) groups
2. Restrained distances
 O1W-H1WB = O1W-H1WA = O2W_$1-H2WA_$1 = O2W_$1-H2WB_$1
 0.8 with sigma of 0.02
 H2WA-H2WB
 1.25 with sigma of 0.04
 H1WB-H1WA
 1.25 with sigma of 0.04
3. Rigid body (RIGU) restrains
 O2A, O2, O3A, O3, S1A, S1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O3A, O2, S1, S1A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O2A)=Sof(O3A)=1-FVAR(1)
 Sof(O2)=Sof(O3)=FVAR(1)
 Sof(S1A)=1-FVAR(2)
 Sof(S1)=FVAR(2)
 Fixed Sof: O3W(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C16(H16), C10(H10), C7(H7A), C8(H8A), C11(H11), C4(H4),
 C13(H13), C17(H17), C6(H6), C18(H18), C23(H23), C21(H21), C26(H26), C25(H25),
 C20(H20), C22(H22)
5.b Idealised tetrahedral OH refined as rotating group:
 O8(H8), O7(H7)
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_olex2_submission_special_instructions 'No special instructions were received'