Synthesis and crystal structure of a new chiral α-aminooxime nickel(II) complex
Homrani, Yasmina; Dahdouh, Abdelaziz; El Amrani, Mohamed Amin; Loxq, Pauline; Capet, Frédéric; Suisse, Isabelle; Sauthier, Mathieu; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021010537

data_2243940
_publ_section_title
;
 Synthesis and crystal structure of a new chiral \a-aminooxime nickel(II)
 complex
;
_journal_coeditor_code           EX2048
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021010537
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_iupac          '[Ni2 Cl2 (C16 H23 Cl N3 O)2]'
_chemical_formula_moiety         'C32 H46 Cl4 N6 Ni2 O2'
_chemical_formula_sum            'C32 H46 Cl4 N6 Ni2 O2'
_chemical_formula_weight         805.97
_chemical_name_systematic
'Dichloridobis{(2<i>S</i>,5<i>R</i>)-2-methyl-5-(prop-1-en-2-yl)-2-[(pyridin-2-yl)methylamino]cyclohexan-1-one oxime}dinickel(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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.014(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3729(9)
_cell_length_b                   8.9363(7)
_cell_length_c                   16.4248(16)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.65
_cell_volume                     1792.9(3)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX2 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT(Bruker, 2019)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42747
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.493
_diffrn_reflns_theta_min         1.357
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.185
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3850 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         10769
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0581P)^2^+0.9636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                9436
_reflns_number_total             10769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2048sup1.cif
_cod_data_source_block           I
_cod_database_code               2243940
_shelx_estimated_absorpt_t_min   0.759
_shelx_estimated_absorpt_t_max   0.851
_shelx_hkl_checksum              30619
_shelx_res_checksum              97173
_cod_database_fobs_code 2243940