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_2241619
_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 (C28 H16 B F2 N4 O4)2 (C14 H10 N2 O2)] , 3C H2 Cl2
;
_chemical_formula_moiety         'C70 H42 B2 F4 N10 Ni3 O10, 3(C H2 Cl2)'
_chemical_formula_sum            'C73 H48 B2 Cl6 F4 N10 Ni3 O10'
_chemical_formula_weight         1456.88
_chemical_name_systematic
;Bis(\m~2~-bis{[10-(oxidoimino)-9,10-dihydrophenanthren-9-ylidene]amino}
difluoroborato)(phenanthrene-9,10-dione dioxime)trinickel(II)
dichloromethane trisolvate
;
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 112.411(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6414(8)
_cell_length_b                   30.8358(11)
_cell_length_c                   14.7380(8)
_cell_measurement_reflns_used    25728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.473
_cell_measurement_theta_min      3.376
_cell_volume                     6571.5(6)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_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
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2940
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type
'Agilent SuperNova Dual Source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25337
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.998
_diffrn_reflns_theta_min         3.376
_exptl_absorpt_coefficient_mu    1.671
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       Block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.825
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         13041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+8.2009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2264
_reflns_number_gt                8782
_reflns_number_total             13041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2575sup1.cif
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_cod_database_code               2241619
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_shelx_res_checksum              68448
_shelx_fab_checksum              19149
_shelxl_version_number           .2013
_cod_database_fobs_code 2241619