Tetra-sodium Nitrilo-tris(methylenephosphonato)-manganate(II) Na4[MnII{N(CH2PO3)3}] 13H2O: Synthesis and Some Structural Features
Somov, N.V.; Chausov, F.F.; Lomova, N.V.; Shumilova, M.A.; Zhirov, D.K.; Crystallography Reports 65 (2020) 233–241; doi:10.1134/S1063774520020224

data_1564832
_publ_section_title
;
 Tetra-sodium Nitrilo-tris(methylenephosphonato)-manganate(II)
 Na4[MnII{N(CH2PO3)3}] 13H2O: Synthesis and Some Structural Features
;
_journal_issue                   2
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              233
_journal_page_last               241
_journal_paper_doi               10.1134/S1063774520020224
_journal_volume                  65
_journal_year                    2020
_chemical_formula_sum            'C3 H32 Mn N Na4 O22 P3'
_chemical_formula_weight         674.1
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2019-01-17T13:17:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.619(3)
_cell_angle_beta                 97.149(3)
_cell_angle_gamma                116.991(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2146(4)
_cell_length_b                   11.2687(4)
_cell_length_c                   12.4625(4)
_cell_measurement_reflns_used    12320
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.468
_cell_measurement_theta_min      3.578
_cell_volume                     1260.47(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0462048
_diffrn_orient_matrix_UB_12      0.0126927
_diffrn_orient_matrix_UB_13      0.0292791
_diffrn_orient_matrix_UB_21      0.0530477
_diffrn_orient_matrix_UB_22      0.035906
_diffrn_orient_matrix_UB_23      0.0560451
_diffrn_orient_matrix_UB_31      0.0256857
_diffrn_orient_matrix_UB_32      0.0681127
_diffrn_orient_matrix_UB_33      -0.0041463
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24974
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.473
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       prism
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0351P)^2^+0.2175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0
_reflns_number_gt                6565
_reflns_number_total             7665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp1u8g01cb
_cod_data_source_block           mnnaatmp
_cod_database_code               1564832