Anion coordination directed synthesis patterns for [Ni4] aggregates: structural changes for thiocyanate coordination and ligand arm hydrolysis
Das, Manisha; Herchel, Radovan; Trávníček, Zdeněk; Bertolasi, Valerio; Ray, Debashis; New Journal of Chemistry 42 (2018) 16717–; doi:10.1039/C8NJ03269F

data_7057714
_publ_section_title
;
 Anion coordination directed synthesis patterns for [Ni4] aggregates:
 structural changes for thiocyanate coordination and ligand arm hydrolysis
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16717
_journal_paper_doi               10.1039/C8NJ03269F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety
'C40 H61 N4 Ni4 O16, (C3 H5 O2), (N O3), (C2 H3 N), (H O), 0.5 O'
_chemical_formula_sum            'C45 H72 N6 Ni4 O22.5'
_chemical_formula_weight         1291.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-05 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                95.105(7)
_cell_angle_beta                 95.350(7)
_cell_angle_gamma                94.242(7)
_cell_formula_units_Z            2
_cell_length_a                   11.186(3)
_cell_length_b                   12.760(4)
_cell_length_c                   19.351(5)
_cell_measurement_reflns_used    33595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.418
_cell_measurement_theta_min      1.062
_cell_volume                     2729.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33595
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.418
_diffrn_reflns_theta_min         1.062
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.985
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         10741
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.09
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+2.4289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9064
_reflns_number_total             10741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03269f2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 7057712--7057715.cif.'
_cod_original_cell_volume        2729.6(13)
_cod_original_formula_sum        'C45 H72 N6 Ni4 O22.50'
_cod_database_code               7057714
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              65469