New homodinuclear tris(3-alkylpyrazolyl)borate complexes of Co^II^ and Ni^II^ with a tetraacetylethane dianion as a bridging ligand
Mikhalyova, Elena A.; Trofimenko, Swiatoslaw; Zeller, Matthias; Addison, Anthony W.; Pavlishchuk, Vitaly V.; Acta Crystallographica Section C 72 (2016) 777–785; doi:10.1107/S205322961601398X

data_2020607
_publ_section_title
;
 New homodinuclear tris(3-alkylpyrazolyl)borate complexes of Co^II^ and
 Ni^II^ with a tetraacetylethane dianion as a bridging ligand
;
_journal_coeditor_code           YP3119
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              777
_journal_page_last               785
_journal_paper_doi               10.1107/S205322961601398X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Ni2 (C24 H40 B N6)2 (C10 H12 O4)]'
_chemical_formula_moiety         'C58 H92 B2 N12 Ni2 O4'
_chemical_formula_sum            'C58 H92 B2 N12 Ni2 O4'
_chemical_formula_weight         1160.47
_chemical_name_systematic
(\m-3,4-Diacetylhexa-2,4-diene-2,5-diolato-\k^4^<i>O</i>^2^,<i>O</i>^3^:<i>O</i>^4^,<i>O</i>^5^)bis{[tris(3-neopentyl-1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)borato]nickel(II)}
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.630(3)
_cell_length_b                   61.387(10)
_cell_length_c                   10.4220(17)
_cell_measurement_reflns_used    2424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.46
_cell_volume                     12559(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and
SHELXLE (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       81
_diffrn_reflns_limit_k_min       -83
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14135
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.481
_diffrn_reflns_theta_min         2.178
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(APEX2; Bruker, 2009)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.252
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1695 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6859
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                6456
_reflns_number_total             6859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3119sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2020606--2020607.cif.'
_cod_database_code               2020607
_cod_database_fobs_code          2020607
_shelx_estimated_absorpt_t_min   0.715
_shelx_estimated_absorpt_t_max   0.892
_shelx_hkl_checksum              46031
_shelx_res_checksum              23815