Direct C-N Coupling in an in Situ Ligand Transformation and the Self-Assembly of a Tetrametallic [Ni(II)4] Staircase.
Ghosh, Aloke Kumar; Singha Mahapatra, Tufan; Clérac, Rodolphe; Mathonière, Corine; Bertolasi, Valerio; Ray, Debashis; Inorganic chemistry 54 (2015) 5136–5138; doi:10.1021/acs.inorgchem.5b00411

data_4343026
_publ_section_title
;
 Direct C-N Coupling in an in Situ Ligand Transformation and the
 Self-Assembly of a Tetrametallic [Ni(II)4] Staircase.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5136
_journal_page_last               5138
_journal_paper_doi               10.1021/acs.inorgchem.5b00411
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C74 H98 N14 Ni4 O12, 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C76 H110 N14 Ni4 O16'
_chemical_formula_weight         1710.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.776(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.342(3)
_cell_length_b                   13.667(3)
_cell_length_c                   24.784(5)
_cell_measurement_reflns_used    33554
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.70
_cell_volume                     4180.1(16)
_computing_cell_refinement       'BRUCKER SMART APEX II'
_computing_data_collection       'BRUCKER SMART APEX II'
_computing_data_reduction        'BRUCKER SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'BRUCKER SMART APEX II CCD'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2014
_diffrn_reflns_av_sigmaI/netI    0.1405
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33554
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1653
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2247
_refine_ls_wR_factor_ref         0.2929
_reflns_number_gt                3686
_reflns_number_total             7029
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic5b00411_si_002.cif
_cod_data_source_block           Complex_1(new)
_cod_depositor_comments          'Adding full bibliography for 4343026.cif.'
_cod_original_cell_volume        4180.1(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4343026