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_7242408
_publ_section_title
;
 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         'C16 H14 Ba N2 O10 S2'
_chemical_formula_sum            'C16 H14 Ba N2 O10 S2'
_chemical_formula_weight         595.75
_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             2020-12-31
_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                 100.403(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8633(18)
_cell_length_b                   17.2055(19)
_cell_length_c                   8.9423(11)
_cell_measurement_reflns_used    3941
_cell_measurement_temperature    296.15(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.37
_cell_volume                     2400.6(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0834
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21507
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.762
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.878
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0790 before and 0.0504 after correction. The Ratio of minimum to maximum transmission is 0.8641. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4372
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0421P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3246
_reflns_number_total             4372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00207d2.cif
_cod_data_source_block           3
_cod_database_code               7242408
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1WA of O1W
 At 1.5 times of:
  All C(H,H) groups, H2 of O2
2. Restrained distances
 O2W-H2WA = O2W-H2WB
 0.8 with sigma of 0.02
 O1W-H1WB
 0.8 with sigma of 0.02
 Ba1-H1WB
 3.1 with sigma of 0.02
 H2WA-H2WB
 1.25 with sigma of 0.04
 H1WB-H1WA
 1.33 with sigma of 0.04
3.a Everything fixed:
 H2WA, H2WB
3.b Aromatic/amide H refined with riding coordinates:
 O1W(H1WA), C5(H5), C7(H7), C11(H11), C8(H8), C10(H10), C13(H13), C12(H12),
 C16(H16), C15(H15)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'