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_7242407
_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         'C42 H42 Co3 N6 O24 S4, 2(H2 O)'
_chemical_formula_sum            'C42 H46 Co3 N6 O26 S4'
_chemical_formula_weight         1355.88
_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   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                75.272(2)
_cell_angle_beta                 89.528(3)
_cell_angle_gamma                66.293(4)
_cell_formula_units_Z            1
_cell_length_a                   9.0487(4)
_cell_length_b                   10.2616(3)
_cell_length_c                   16.0633(4)
_cell_measurement_reflns_used    8416
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      76.5720
_cell_measurement_theta_min      4.8780
_cell_volume                     1313.35(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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    'olex2.solve 1.3-beta (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9639
_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    -75.00  16.00   0.50    3.84    --  -38.50 103.00 -32.00  182
  2  \w     22.00  47.00   0.50    3.84    --   49.31-103.00-134.00   50
  3  \w    138.00 163.00   0.50   15.34    --  106.38 103.00 -32.00   50
  4  \w     57.00  98.00   0.50   15.34    --  106.38-103.00-134.00   82
  5  \w    -91.00 -40.00   0.50    3.84    --  -38.50 -37.00  90.00  102
  6  \w   -101.00 -74.00   0.50    3.84    --  -38.50 -77.00-120.00   54
  7  \w    -65.00 -13.00   0.50    3.84    --  -38.50 125.00 150.00  104
  8  \w    -72.00 -15.00   0.50    3.84    --  -38.50 -77.00-120.00  114
  9  \w     -9.00  41.00   0.50    3.84    --   49.31 -37.00   0.00  100
 10  \w    -13.00  61.00   0.50    3.84    --   49.31 -57.00  90.00  148
 11  \w     38.00 112.00   0.50    3.84    --   49.31  57.00-150.00  148
 12  \w     79.00 111.00   0.50   15.34    --  106.38-125.00-180.00   64
 13  \w     44.00 115.00   0.50   15.34    --  106.38 -15.00 -90.00  142
 14  \w     62.00  89.00   0.50   15.34    --  106.38 -94.00  30.00   54
 15  \w     46.00 107.00   0.50   15.34    --  106.38 -30.00  90.00  122
 16  \w     42.00 111.00   0.50   15.34    --  106.38 -45.00 -60.00  138
 17  \w     91.00 117.00   0.50   15.34    --  106.38-125.00 -60.00   52
 18  \w     84.00 130.00   0.50   15.34    --  106.38 -77.00-150.00   92
 19  \w     43.00  73.00   0.50   15.34    --  106.38 -77.00-150.00   60
 20  \w     59.00 110.00   0.50   15.34    --  106.38 -45.00  60.00  102
 21  \w     91.00 149.00   0.50   15.34    --  106.38  77.00 -60.00  116
 22  \w     54.00  81.00   0.50   15.34    --  106.38 -30.00   0.00   54
 23  \w     51.00 107.00   0.50   15.34    --  106.38 -61.00  30.00  112
 24  \w     91.00 122.00   0.50   15.34    --  106.38-125.00 -30.00   62
 25  \w     46.00  96.00   0.50   15.34    --  106.38 -61.00 -60.00  100
 26  \w    110.00 164.00   0.50   15.34    --  106.38  45.00  90.00  108
 27  \w     50.00 115.00   0.50   15.34    --  106.38 -15.00 120.00  130
 28  \w     43.00 117.00   0.50   15.34    --  106.38-125.00  90.00  148
 29  \w     44.00  99.00   0.50   15.34    --  106.38 -45.00-150.00  110
 30  \w     44.00  84.00   0.50   15.34    --  106.38-125.00 -60.00   80
 31  \w    111.00 157.00   0.50   15.34    --  106.38  30.00 120.00   92
 32  \w     77.00 102.00   0.50   15.34    --  106.38 -45.00   0.00   50
 33  \w    104.00 165.00   0.50   15.34    --  106.38  30.00-120.00  122
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1746253000
_diffrn_orient_matrix_UB_12      -0.0136411000
_diffrn_orient_matrix_UB_13      0.0130997000
_diffrn_orient_matrix_UB_21      0.0213589000
_diffrn_orient_matrix_UB_22      -0.0014202000
_diffrn_orient_matrix_UB_23      -0.0950585000
_diffrn_orient_matrix_UB_31      -0.0633941000
_diffrn_orient_matrix_UB_32      0.1699400000
_diffrn_orient_matrix_UB_33      -0.0271615000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11712
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         5.573
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             693
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.655
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4603
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0852
_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^)+(0.1912P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2365
_refine_ls_wR_factor_ref         0.2435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4010
_reflns_number_total             4603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00207d2.cif
_cod_data_source_block           2
_cod_database_code               7242407
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H11 N11 O22 Na11 S11 Co11 '
_shelx_estimated_absorpt_t_max   0.248
_shelx_estimated_absorpt_t_min   0.196
_diffrn_oxdiff_ac3_digest_frames
;
0117657666072fbf4f9e0f2169e55487d3000265c44
;
_diffrn_oxdiff_ac3_digest_hkl
;
019471f5befecb1a3362412448d71d2b28e271
;
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H,H) groups
2. Restrained distances
 O2W-H2WB = O2W-H2WA
 0.8 with sigma of 0.02
 H2WA-H2WB
 1.25 with sigma of 0.04
 Co2-H4WA \\sim Co2-H4WB
 with sigma of 0.02
3.a Free rotating group:
 O4W(H4WA,H4WB), O5W(H5WA,H5WB)
3.b Rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O2W(H2WA)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C10(H10), C8(H8), C7(H7), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21)
;
_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 5.208
_oxdiff_exptl_absorpt_empirical_full_min 0.233