Synthesis, Structure, and Properties of Nickel Complexes with Nitrilotris(methylenephosphonic acid) [Ni(H2O)3N(CH2PO3H)3] and Na4[Ni(H2O)N(CH2PO3)3] 11H2O
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Fedotova, I.V.; Crystallography Reports 61 (2016) 216–224; doi:10.1134/S1063774516020243

data_1564818
_publ_section_title
;
 Synthesis, Structure, and Properties of Nickel Complexes with
 Nitrilotris(methylenephosphonic acid) [Ni(H2O)3N(CH2PO3H)3] and
 Na4[Ni(H2O)N(CH2PO3)3] 11H2O
;
_journal_issue                   2
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              216
_journal_page_last               224
_journal_paper_doi               10.1134/S1063774516020243
_journal_volume                  61
_journal_year                    2016
_chemical_formula_sum            'C3 H16 N Ni O12 P3'
_chemical_formula_weight         409.79
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2015-02-20T15:21:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 115.830(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.17120(10)
_cell_length_b                   16.05700(10)
_cell_length_c                   9.70890(10)
_cell_measurement_reflns_used    17059
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.632
_cell_measurement_theta_min      3.578
_cell_volume                     1286.91(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0302
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0299181
_diffrn_orient_matrix_UB_12      -0.0412752
_diffrn_orient_matrix_UB_13      -0.017764
_diffrn_orient_matrix_UB_21      -0.0265959
_diffrn_orient_matrix_UB_22      0.0017483
_diffrn_orient_matrix_UB_23      0.0584757
_diffrn_orient_matrix_UB_31      -0.0760131
_diffrn_orient_matrix_UB_32      0.0156344
_diffrn_orient_matrix_UB_33      -0.0534335
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43300
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.978
_diffrn_reflns_theta_min         3.446
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.944
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.1424
_exptl_crystal_size_mid          0.1288
_exptl_crystal_size_min          0.0862
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         6734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.5795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0
_reflns_number_gt                5843
_reflns_number_total             6734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp9c5xk4kl
_cod_data_source_block           ni(ii)_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564818