Complex formation of copper(ii), nickel(ii) and zinc(ii) with ethylophosphonoacetohydroxamic acid: solution speciation, synthesis and structural characterization
Ostrowska, Malgorzata; Golenya, Irina A.; Haukka, Matti; Fritsky, Igor O.; Gumienna-Kontecka, Elzbieta; New Journal of Chemistry 43 (2019) 10237–; doi:10.1039/C9NJ01175G

data_7058393
_publ_section_title
;
 Complex formation of copper(ii), nickel(ii) and zinc(ii) with
 ethylophosphonoacetohydroxamic acid: solution speciation, synthesis and
 structural characterization
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10237
_journal_paper_doi               10.1039/C9NJ01175G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C20 H46 Cu5 N4 Na4 O30 P4, 1.5(H2 O)'
_chemical_formula_sum            'C20 H49 Cu5 N4 Na4 O31.5 P4'
_chemical_formula_weight         1383.17
_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
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-03-05 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                91.4700(10)
_cell_angle_beta                 99.1550(10)
_cell_angle_gamma                91.9430(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5160(3)
_cell_length_b                   13.9940(3)
_cell_length_c                   14.6740(2)
_cell_measurement_reflns_used    23641
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2332.17(9)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1e (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         2.565
_exptl_absorpt_coefficient_mu    2.518
_exptl_absorpt_correction_T_max  0.7945
_exptl_absorpt_correction_T_min  0.5963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description       needle
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.951
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         10669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0491P)^2^+7.2260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8022
_reflns_number_total             10669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01175g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
Adding full bibliography for 7058393--7058394.cif.

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H98 Cu10 N8 Na8 O63 P8'
_cod_original_formula_weight         2766.34
_cod_original_formula_moiety         '2(C20 H46 Cu5 N4 Na4 O30 P4), 3(H2 O)'
_cod_original_formula_units_Z            1
_cod_database_code               7058393
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.609
_shelx_estimated_absorpt_t_max   0.811
_shelx_res_checksum              64566