The Trisodium Monohydrogen-Nitrilo-Tris-Methylenephosphonato-Hydroxylaminato-Nitrosyl-Molybdate Octahydrate Na3[Mo(NO)(NH2O){N(CH2PO3)3H}] 8H2O: Synthesis, Structure, and Nature of Coordination Bond of Transition Metal with Non-Innocent Ligand
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Fedotova, I.V.; Lomova, N.V.; Shabanova, I.N.; Petrov, V.G.; Shumilova, M.A.; Zhirov, D.K.; Russian Journal of Coordination Chemistry 43 (2017) 864–873; doi:10.1134/S1070328417120090

data_1564827
_publ_section_title
;
 The Trisodium
 Monohydrogen-Nitrilo-Tris-Methylenephosphonato-Hydroxylaminato-Nitrosyl-Molybdate
 Octahydrate Na3[Mo(NO)(NH2O){N(CH2PO3)3H}] 8H2O: Synthesis, Structure,
 and Nature of Coordination Bond of Transition Metal with Non-Innocent
 Ligand
;
_journal_issue                   12
_journal_name_full
;
 Russian Journal of Coordination Chemistry
;
_journal_page_first              864
_journal_page_last               873
_journal_paper_doi               10.1134/S1070328417120090
_journal_volume                  43
_journal_year                    2017
_chemical_formula_sum            'C3 H25 Mo N3 Na3 O19 P3'
_chemical_formula_weight         665.08
_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             2017-04-12T15:54:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.7060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7385(2)
_cell_length_b                   10.2542(2)
_cell_length_c                   21.6517(3)
_cell_measurement_reflns_used    22433
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.967
_cell_measurement_theta_min      3.755
_cell_volume                     2157.63(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_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      0.00619
_diffrn_orient_matrix_UB_12      0.0642917
_diffrn_orient_matrix_UB_13      0.01191
_diffrn_orient_matrix_UB_21      -0.0006163
_diffrn_orient_matrix_UB_22      -0.0248227
_diffrn_orient_matrix_UB_23      0.0305699
_diffrn_orient_matrix_UB_31      0.072725
_diffrn_orient_matrix_UB_32      -0.0056534
_diffrn_orient_matrix_UB_33      0.0013464
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44025
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.52
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6578
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+2.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.059
_reflns_Friedel_coverage         0
_reflns_number_gt                6095
_reflns_number_total             6578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmpkg0ntwsp
_cod_data_source_block           moatmp
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564827