Trinuclear nickel coordination complexes of phenanthrene-9,10-dione dioxime
Williams, Owen M.; Cowley, Alan H.; Acta Crystallographica Section E 72 (2016) 538–542; doi:10.1107/S2056989016004023

data_2241618
_publ_section_title
;
 Trinuclear nickel coordination complexes of phenanthrene-9,10-dione
 dioxime
;
_journal_coeditor_code           PK2575
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              538
_journal_page_last               542
_journal_paper_doi               10.1107/S2056989016004023
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
;
[Ni3 (C14 H8 N2 O2)2 (C14 H9 N2 O2)2 (C14 H10 N2 O2)] , 2C7 H8
;
_chemical_formula_moiety         'C70 H44 N10 Ni3 O10, 2(C7 H8)'
_chemical_formula_sum            'C84 H60 N10 Ni3 O10'
_chemical_formula_weight         1545.55
_chemical_name_systematic
;Bis[\m~2~-9,10-bis(oxidoimino)phenanthrene]bis[\m~2~-10-(oxidoimino)phenanthrene-9-one oxime](phenanthrene-9,10-dione
dioxime)trinickel(II) toluene disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.000
_cell_angle_beta                 101.757(4)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   15.973(3)
_cell_length_b                   18.639(3)
_cell_length_c                   22.785(4)
_cell_measurement_reflns_used    20424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0999
_cell_measurement_theta_min      1.3022
_cell_volume                     6641(2)
_computing_cell_refinement
;
CrystalClear (Rigaku Inc, 2008)
;
_computing_data_collection
;
CrystalClear (Rigaku Inc, 2008)
;
_computing_data_reduction
;
CrystalClear (Rigaku Inc, 2008)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010) and WinGX (Farrugia, 1999)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79592
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.799
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       Block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.1580
_exptl_crystal_size_mid          0.1110
_exptl_crystal_size_min          0.1060
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.680
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         15260
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+7.4732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                13993
_reflns_number_total             15260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2575sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        6641.1(19)
_cod_database_code               2241618
_shelx_hkl_checksum              56600
_shelx_res_checksum              12996
_shelxl_version_number           .2013
_cod_database_fobs_code 2241618