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_7235281
_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
'C94 H67 N18 Ni5 O13, Cl O4, 8.8(C H4 O), 1.4(H2 O)'
_chemical_formula_sum            'C102.8 H105 Cl N18 Ni5 O27.2'
_chemical_formula_weight         2356.85
_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                93.80(3)
_cell_angle_beta                 100.35(3)
_cell_angle_gamma                97.00(3)
_cell_formula_units_Z            2
_cell_length_a                   15.782(4)
_cell_length_b                   17.617(5)
_cell_length_c                   19.885(5)
_cell_measurement_reflns_used    19308
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      2.75
_cell_volume                     5376(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      80(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.874
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64959
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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            pink
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2445
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1492
_refine_ls_number_reflns         24669
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0981P)^2^+15.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                16776
_reflns_number_total             24669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41455h.cif
_cod_data_source_block           at594bba
_cod_original_cell_volume        5376(2)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C102.80 H105 Cl N18 Ni5 O27.20'
_cod_database_code               7235281