Monoanionic salicylaldimine ligands with (thio)phosphoryl pendant arms: Synthesis and complexing features
Diana V. Aleksanyan; Valentina Yu. Aleksenko; Yulia V. Nelyubina; Andrei A. Vasil-ev; Rinat R. Aysin; Zinaida S. Klemenkova; Vladimir A. Kozlov; Pavel V. Petrovskii; Irina L. Odinets; Inorganica Chimica Acta 404 (2013) 167–174; doi:

data_1517766
_publ_section_title
;
 Monoanionic salicylaldimine ligands with (thio)phosphoryl pendant arms:
 Synthesis and complexing features
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              167
_journal_page_last               174
_journal_volume                  404
_journal_year                    2013
_chemical_formula_moiety         'C50 H38 N2 Ni O4 P2, 2(C2 H6 O), 2(H2 O)'
_chemical_formula_sum            'C54 H54 N2 Ni O8 P2'
_chemical_formula_weight         979.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                61.711(3)
_cell_angle_beta                 76.080(2)
_cell_angle_gamma                85.684(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4396(9)
_cell_length_b                   11.8274(11)
_cell_length_c                   12.3009(11)
_cell_measurement_reflns_used    2702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1172.60(19)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            13030
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5662
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.3376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                3872
_reflns_number_total             5662
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ICA-2013-404-167-174-5.cif
_cod_data_source_block           4
_cod_database_code               1517766