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_7058501
_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
'C26 H33 N2 Ni2 O8 S2, C2 H8 N O, H2 O [+ solvent'
_chemical_formula_sum            'C28 H43 N3 Ni2 O10 S2'
_chemical_formula_weight         763.15
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-06-13
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-06-17 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            3
_cell_length_a                   17.5135(5)
_cell_length_b                   17.5135(5)
_cell_length_c                   10.5236(3)
_cell_measurement_reflns_used    9401
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1940
_cell_measurement_theta_min      3.5470
_cell_volume                     2795.38(14)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12217
_diffrn_reflns_point_group_measured_fraction_full 0.775
_diffrn_reflns_point_group_measured_fraction_max 0.700
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.396
_diffrn_reflns_theta_min         3.311
_diffrn_source                   'microfocus sealed tube X-ray'
_diffrn_source_type              'supernova Mo X-ray'
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_transmission_factor_max   0.800
_exptl_transmission_factor_min   0.702
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 1728 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5963
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0599
_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^)+(0.1065P)^2^+5.6584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.504
_reflns_Friedel_fraction_full    0.553
_reflns_Friedel_fraction_max     0.469
_reflns_number_gt                5340
_reflns_number_total             5963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02573a2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7058499--7058502.cif.'
_cod_original_cell_volume        2795.38(18)
_cod_database_code               7058501
_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. Restrained distances
 O2-H10A
 2.8 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O10(H10A,H10B)
4.b Ternary CH refined with riding coordinates:
 N2(H2), N1(H1), C14(H14), C2(H2A)
4.c Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C27(H27A,H27B), C6(H6A,H6B), C16(H16A,H16B), C3(H3A,H3B),
 C4(H4A,H4B), C15(H15A,H15B), C28(H28A,H28B)
4.d Me refined with riding coordinates:
 C26(H26A,H26B,H26C)
4.e Aromatic/amide H refined with riding coordinates:
 C21(H21), C9(H9), C12(H12), C11(H11), C10(H10), C24(H24), C22(H22), C23(H23)
4.f Idealised Me refined as rotating group:
 N3(H3C,H3D,H3E), C17(H17A,H17B,H17C), C5(H5A,H5B,H5C)
4.g Idealised tetrahedral OH refined as rotating group:
 O9(H9A)
;
_olex2_submission_special_instructions 'No special instructions were received'