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_7058500
_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_formula_moiety         'C29 H40 N3 Ni2 O9 S2, C2 H8 N O, 2(H2 O)'
_chemical_formula_sum            'C31 H52 N4 Ni2 O12 S2'
_chemical_formula_weight         854.30
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   10.60766(15)
_cell_length_b                   10.60766(15)
_cell_length_c                   34.4981(8)
_cell_measurement_reflns_used    21054
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2280
_cell_measurement_theta_min      3.5070
_cell_volume                     3881.81(12)
_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 0.994
_diffrn_measured_fraction_theta_max 0.944
_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    -59.00  -1.00   0.50   15.00    --   -9.91 -38.00-128.00  116
  2  \w    -45.00   7.00   0.50   15.00    --   -9.91 113.00 105.00  104
  3  \w     -3.00  49.00   0.50   15.00    --   10.22-113.00  13.00  104
  4  \w     28.00  54.00   0.50   15.00    --   -9.91  77.00-180.00   52
  5  \w    -35.00  -3.00   0.50   15.00    --   -9.91 125.00 -30.00   64
  6  \w    -35.00  22.00   0.50   15.00    --   -9.91  77.00-180.00  114
  7  \w      3.00  28.00   0.50   15.00    --   10.22  87.00-146.00   50
  8  \w    -60.00  21.00   0.50   15.00    --   10.22 -19.00  60.00  162
;
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            27372
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.409
_diffrn_reflns_theta_min         3.243
_diffrn_source                   'microfocused sealed tube X-ray'
_diffrn_source_type              'supernova Mo X-ray'
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76087
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_recrystallization_method slowevaporation
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2432 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7052
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0325P)^2^+2.8695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.728
_reflns_Friedel_fraction_max     0.644
_reflns_number_gt                6581
_reflns_number_total             7052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02573a2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7058499--7058502.cif.'
_cod_original_cell_volume        3881.81(14)
_cod_database_code               7058500
_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, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O12(H12A,H12B)
2.b Ternary CH refined with riding coordinates:
 N2(H2), N1(H1), C2(H2A), C14(H14)
2.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C3(H3A,H3B), C6(H6A,H6B), C15(H15A,H15B), C30(H30A,H30B),
 C4(H4A,H4B), C16(H16A,H16B), C31(H31A,H31B)
2.d Aromatic/amide H refined with riding coordinates:
 C27(H27), C9(H9), C21(H21), C24(H24), C12(H12), C23(H23), C22(H22), C11(H11),
 C10(H10)
2.e Idealised Me refined as rotating group:
 N4(H4C,H4D,H4E), C26(H26A,H26B,H26C), C17(H17A,H17B,H17C), C29(H29A,H29B,
 H29C), C28(H28A,H28B,H28C), C5(H5A,H5B,H5C)
2.f Idealised tetrahedral OH refined as rotating group:
 O10(H10A)
;
_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
;