An indeno-quinoxaline based oxime ligand for the synthesis of polynuclear Ni(ii) clusters
Canaj, Angelos B.; Nodaraki, Lydia E.; Philippidis, Aggelos; Tzimopoulos, Demetrios I.; Fotopoulou, Eirini; Siczek, Milosz; Lis, Tadeusz; Milios, Constantinos J.; RSC Advances 3 (2013) 13214–; doi:10.1039/c3ra41455h

data_7235279
_publ_section_title
;
 An indeno-quinoxaline based oxime ligand for the synthesis of polynuclear
 Ni(ii) clusters
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              13214
_journal_paper_doi               10.1039/c3ra41455h
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety
'(C78 H47 N15 Ni3 O8), 2.6(C2 H3 N), 0.7(C H4 O), 0.2(O H2)'
_chemical_formula_sum            'C83.9 H58 N17.6 Ni3 O8.9'
_chemical_formula_weight         1631.21
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.02(5)
_cell_angle_beta                 88.64(5)
_cell_angle_gamma                73.41(5)
_cell_formula_units_Z            2
_cell_length_a                   14.565(7)
_cell_length_b                   15.905(7)
_cell_length_c                   16.366(8)
_cell_measurement_reflns_used    1154
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      2.66
_cell_volume                     3620(3)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'Xcalibur PX with Ruby CCD'
_diffrn_measurement_method       /w
_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  0.2439
_diffrn_reflns_av_sigmaI/netI    0.7201
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32324
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a
multifaceted crystal model based on expressions
derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         16398
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.4374
_refine_ls_R_factor_gt           0.1214
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.2189
_reflns_number_gt                3667
_reflns_number_total             16398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41455h.cif
_cod_data_source_block           at586a
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C83.90 H58 N17.60 Ni3 O8.90'
_cod_database_code               7235279