Crystal structure of bis(bis{(<i>E</i>)-[(6-{(<i>E</i>)-[(4-fluorobenzyl)imino]methyl}pyridin-2-yl)methylidene](4-fluorophenyl)amine}nickel(II)) tetrabromide nonahydrate
Basaran, Ismet; Rhaman, Md Mhahabubur; Powell, Douglas R.; Hossain, Md. Alamgir; Acta Crystallographica Section E 71 (2015) m226–m227; doi:10.1107/S2056989015021519

data_2241351
_publ_section_title
;
 Crystal structure of
 bis(bis{(<i>E</i>)-[(6-{(<i>E</i>)-[(4-fluorobenzyl)imino]methyl}pyridin-2-yl)methylidene](4-fluorophenyl)amine}nickel(II))
 tetrabromide nonahydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m226
_journal_page_last               m227
_journal_paper_doi               10.1107/S2056989015021519
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (C21 H17 F2 N3)2]2 Br4, 9H2 O'
_chemical_formula_moiety         'C42 H34 F4 N6 Ni, 2(Br -), 4.5(H2 O)'
_chemical_formula_sum            'C42 H43 Br2 F4 N6 Ni O4.5'
_chemical_formula_weight         998.35
_chemical_name_systematic
;Bis(bis{(<i>E</i>)-[(6-{(<i>E</i>)-[(4-fluorobenzyl)imino]methyl}pyridin-2-yl)methylidene](4-fluorophenyl)amine}nickel(II)) tetrabromide
nonahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                87.377(2)
_cell_angle_beta                 86.955(2)
_cell_angle_gamma                72.339(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1000(16)
_cell_length_b                   12.5686(16)
_cell_length_c                   29.149(4)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      2.24
_cell_volume                     4216.0(10)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            94344
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         1.400
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.774
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         19210
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                15090
_reflns_number_total             19210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fk2092sup1.cif
_cod_data_source_block           I
_cod_database_code               2241351
_cod_database_fobs_code          2241351
_shelx_estimated_absorpt_t_min   0.571
_shelx_estimated_absorpt_t_max   0.760
_shelx_hkl_checksum              86727
_shelx_res_checksum              62989