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_7235282
_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
'C122 H91.5 N25.5 Ni7 O16.5, 2(Cl O4), 4(C2 H3 N), 0.25(H2 O)'
_chemical_formula_sum            'C130 H104 Cl2 N29.5 Ni7 O24.75'
_chemical_formula_weight         2953.30
_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                96.06(3)
_cell_angle_beta                 106.28(3)
_cell_angle_gamma                101.89(3)
_cell_formula_units_Z            2
_cell_length_a                   18.314(7)
_cell_length_b                   18.903(6)
_cell_length_c                   19.287(6)
_cell_measurement_reflns_used    5922
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.73
_cell_volume                     6176(4)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,2008'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,2008'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Xcalibur 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  0.0964
_diffrn_reflns_av_sigmaI/netI    0.2027
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61933
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.80
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
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    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3033
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1818
_refine_ls_number_reflns         28103
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.2127
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1914
_reflns_number_gt                12546
_reflns_number_total             28103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41455h.cif
_cod_data_source_block           at639a
_cod_original_cell_volume        6174(4)
_cod_original_sg_symbol_Hall     -p1
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C130 H104 Cl2 N29.50 Ni7 O24.75'
_cod_database_code               7235282