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_7235280
_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
'C100 H66 N18 Ni6 O16, 1.5(C H4 O), 1.3(H2 O)'
_chemical_formula_sum            'C101.5 H74.6 N18 Ni6 O18.8'
_chemical_formula_weight         2199.45
_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                64.27(4)
_cell_angle_beta                 77.69(3)
_cell_angle_gamma                63.98(4)
_cell_formula_units_Z            2
_cell_length_a                   17.036(7)
_cell_length_b                   17.422(7)
_cell_length_c                   19.400(8)
_cell_measurement_reflns_used    5885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.79
_cell_volume                     4659(4)
_computing_cell_refinement       'CrysAlis RED, Agilent Technologies, 2010'
_computing_data_collection       'CrysAlis CCD, Agilent Technologies, 2010'
_computing_data_reduction        'CrysAlis RED, Agilent Technologies, 2010'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KM4CCD
_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  0.1044
_diffrn_reflns_av_sigmaI/netI    0.2869
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35182
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Agilent Technologies, 2010
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            red
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1334
_refine_ls_number_reflns         17223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.2115
_refine_ls_R_factor_gt           0.0562
_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^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0599
_reflns_number_gt                5626
_reflns_number_total             17223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41455h.cif
_cod_data_source_block           at488a
_cod_original_cell_volume        4659(3)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C101.50 H74.60 N18 Ni6 O18.80'
_cod_database_code               7235280