Crystal structure of an unknown solvate of bis(tetra-<i>n</i>-butylammonium) [<i>N</i>,<i>N</i>'-(4-trifluoromethyl-1,2-phenylene)bis(oxamato)-κ^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>']nickelate(II)
Eya'ane Meva, François; Schaarschmidt, Dieter; Rüffer, Tobias; Acta Crystallographica Section E 71 (2015) 578–581; doi:10.1107/S205698901500835X

data_2240674
_publ_section_title
;
 Crystal structure of an unknown solvate of
 bis(tetra-<i>n</i>-butylammonium)
 [<i>N</i>,<i>N</i>'-(4-trifluoromethyl-1,2-phenylene)bis(oxamato)-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>']nickelate(II)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              578
_journal_page_last               581
_journal_paper_doi               10.1107/S205698901500835X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C16 H36 N)2 [Ni (C11 H3 F3 N2 O6)]'
_chemical_formula_moiety         '2(C16 H36 N +), C11 H3 F3 N2 Ni O6 2-'
_chemical_formula_sum            'C43 H75 F3 N4 Ni O6'
_chemical_formula_weight         859.78
_chemical_name_systematic
;Bis(tetra-<i>n</i>-butylammonium)
[<i>N</i>,<i>N</i>'-(4-trifluoromethyl-1,2-phenylene)bis(oxamato)-\k^4^<i>O</i>,<i>N</i>,<i>N</i>',<i>O</i>']nickelate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.136(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5285(3)
_cell_length_b                   17.3370(3)
_cell_length_c                   14.1484(3)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    110
_cell_measurement_theta_max      60.3930
_cell_measurement_theta_min      4.5270
_cell_volume                     4786.83(15)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012), SHELXTL (Sheldrick, 2008)
and PLATON
(Spek, 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and
<i>SQUEEZE</i> (Spek, 2015)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Oxford Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15600
_diffrn_reflns_theta_full        60.500
_diffrn_reflns_theta_max         60.470
_diffrn_reflns_theta_min         3.410
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 25
_diffrn_standards_interval_time  50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis RED</i>; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0577P)^2^+2.8029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                3142
_reflns_number_total             3545
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5144sup1.cf
_cod_data_source_block           I
_cod_database_code               2240674
_shelx_hkl_checksum              68595
_shelx_res_checksum              28374
_shelx_fab_checksum              64320
_shelxl_version_number           .2013
_cod_database_fobs_code 2240674