The role of a weakly coordinating thioether group in ligation controlled molecular self-assemblies and their inter-conversions in Ni(ii) complexes of l-methionine derived ligand
Kumar, Rakesh; Mutreja, Vishal; Sharma, Gyaneshwar; Kumar, Sanjeev; Ali, Anzar; Mehta, S. K.; Venugopalan, P.; Kataria, Ramesh; Sahoo, Subash Chandra; New Journal of Chemistry 43 (2019) 11222–; doi:10.1039/C9NJ02573A

data_7058499
_publ_section_title
;
 The role of a weakly coordinating thioether group in ligation controlled
 molecular self-assemblies and their inter-conversions in Ni(ii) complexes
 of l-methionine derived ligand
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11222
_journal_paper_doi               10.1039/C9NJ02573A
_journal_volume                  43
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_compound_source        synstehsized
_chemical_formula_moiety         '3(C12 H16 N Ni0.5 O3 S)'
_chemical_formula_sum            'C36 H48 N3 Ni1.5 O9 S3'
_chemical_formula_weight         851.02
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-30
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-05-09 deposited with the CCDC.    2019-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   14.1696(4)
_cell_length_b                   14.1696(4)
_cell_length_c                   12.1596(4)
_cell_measurement_reflns_used    6382
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3080
_cell_measurement_theta_min      3.3170
_cell_volume                     2114.29(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_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    -11.00  22.00   0.50   30.00    --   -9.91 -95.00  41.00   66
  2  \w     40.00  73.00   0.50   30.00    --   10.22-148.00 -97.00   66
  3  \w    -53.00  -5.00   0.50   30.00    --   -9.91 125.00-150.00   96
  4  \w    -43.00 -14.00   0.50   30.00    --   -9.91 125.00 -90.00   58
  5  \w    -22.00  60.00   0.50   30.00    --   -9.91  19.00  90.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8856
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.317
_diffrn_reflns_theta_min         3.320
_diffrn_source                   'microfocused sealed tube X-ray'
_diffrn_source_type              'supernova Mo X-ray'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colour
_exptl_crystal_density_diffrn    0.668
_exptl_crystal_description       rod
_exptl_crystal_F_000             447
_exptl_crystal_recrystallization_method slowevaporation
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 989 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0595P)^2^+0.0926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                2611
_reflns_number_total             2998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02573a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7058499--7058502.cif.'
_cod_original_cell_volume        2114.29(13)
_cod_original_formula_sum        'C36 H48 N3 Ni1.50 O9 S3'
_cod_database_code               7058499
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Ni1(0.25) S1(0.5) N1(0.5) H1(0.5) O3(0.5) O2(0.5) O1(0.5) C7(0.5)
 C8(0.5) C2(0.5) H2(0.5) C6(0.5) H6A(0.5) H6B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C3(0.5) H3A(0.5) H3B(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5) C9(0.5) H9(0.5) C1(0.5) C12(0.5) H12(0.5) H3(0.5)
3.a Ternary CH refined with riding coordinates:
 N1(H1), C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C9(H9), C12(H12)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_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
;