Synthesis and crystal structure of a disubstituted nickel(II) bis[(dimethylaminophenylimino)ethyl]pyridine chloride complex
Matthews, Morgan; Sendzik, Madison; Bruggeman, Adrienne; Kearns, Claire; Oliver, Allen G.; Babbini, Dominic C.; Acta Crystallographica Section E 73 (2017) 1167–1171; doi:10.1107/S2056989017010088

data_2242163
_publ_section_title
;
 Synthesis and crystal structure of a disubstituted nickel(II)
 bis[(dimethylaminophenylimino)ethyl]pyridine chloride complex
;
_journal_coeditor_code           WM5402
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1167
_journal_page_last               1171
_journal_paper_doi               10.1107/S2056989017010088
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ni (C25 H29 N5)2] Cl2, 2C H2 Cl2, 2H2 O'
_chemical_formula_moiety
'C50 H58 N10 Ni 2+, 2(Cl -), 2(C H2 Cl2), 2(H2 O)'
_chemical_formula_sum            'C52 H66 Cl6 N10 Ni O2'
_chemical_formula_weight         1134.55
_chemical_name_systematic
'Bis[2,6-bis(1-{[4-(dimethylamino)phenyl]imino-\k<i>N</i>}ethyl)pyridine-\k<i>N</i>]nickel dichloride--dichloromethane--water (1/2/2)'
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                79.6276(12)
_cell_angle_beta                 81.2551(12)
_cell_angle_gamma                89.3481(12)
_cell_formula_units_Z            4
_cell_length_a                   13.2227(5)
_cell_length_b                   17.7311(6)
_cell_length_c                   24.0242(9)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.27
_cell_volume                     5475.4(3)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006) and POV-Ray (Cason, 2003)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa X8 APEXII'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69305
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.190
_diffrn_reflns_theta_min         0.872
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.9173
_exptl_absorpt_correction_T_min  0.8231
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.152
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.002
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         24260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0506P)^2^+2.6902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                17532
_reflns_number_total             24260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5402sup1.cif
_cod_data_source_block           I
_cod_database_code               2242163
_cod_database_fobs_code          2242163
_shelx_estimated_absorpt_t_min   0.818
_shelx_estimated_absorpt_t_max   0.901
_shelx_hkl_checksum              96953
_shelx_res_checksum              16262