Crystal structures of a copper(II) and the isotypic nickel(II) and palladium(II) complexes of the ligand (<i>E</i>)-1-[(2,4,6-tribromophenyl)diazenyl]naphthalen-2-ol
Chetioui, Souheyla; Rouag, Djamil-Azzeddine; Djukic, Jean-Pierre; Bochet, Christian G.; Touzani, Rachid; Bailly, Corinne; Crochet, Aurélien; Fromm, Katharina M.; Acta Crystallographica Section E 72 (2016) 1093–1098; doi:10.1107/S205698901601080X

data_2241763
_publ_section_title
;
 Crystal structures of a copper(II) and the isotypic nickel(II) and
 palladium(II) complexes of the ligand
 (<i>E</i>)-1-[(2,4,6-tribromophenyl)diazenyl]naphthalen-2-ol
;
_journal_coeditor_code           SU5299
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1093
_journal_page_last               1098
_journal_paper_doi               10.1107/S205698901601080X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cu (C16 H8 Br3 N2 O)2]'
_chemical_formula_moiety         'C32 H16 Br6 Cu N4 O2'
_chemical_formula_sum            'C32 H16 Br6 Cu N4 O2'
_chemical_formula_weight         1031.49
_chemical_name_systematic
;
Bis{(<i>E</i>)-1-[(2,4,6-tribromophenyl)diazenyl]naphthalen-2-olato}copper(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.032(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9423(7)
_cell_length_b                   12.1314(10)
_cell_length_c                   12.8974(10)
_cell_measurement_reflns_used    19031
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1786.6(2)
_computing_cell_refinement
;
Denzo (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
Denzo (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         2.355
_exptl_absorpt_coefficient_mu    7.355
_exptl_absorpt_correction_T_max  0.38570
_exptl_absorpt_correction_T_min  0.31075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(MULABS; Spek, 2009)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             982
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The residual electron density was assigned to two molecules of the
dichloromethane [179/2 = 89e per asymmetric unit].
This is equivalent to two molecules of CH2Cl2,
which would give 84e.
;
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.580
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1648 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.006(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7819
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                4785
_reflns_number_total             7819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5299sup1.cif
_cod_data_source_block           I
_cod_database_code               2241763
_shelx_hkl_checksum              60977
_shelx_res_checksum              68259
_shelxl_version_number           .2013
_cod_database_fobs_code 2241763