Aquanitrilotris(methylenephosphonato)dirubidium [Rb2(H2O){12-NH(CH2PO3H)3}]: Synthesis and Structure
Somov, N.V.; Chausov, F.F.; Zakirova, R.M.; Shumilova, M.A.; Aleksandrov, V.A.; Petrov, V.G.; Crystallography Reports 62 (2017) 734–738; doi:10.1134/S1063774517050212

data_1564825
_publ_section_title
;
 Aquanitrilotris(methylenephosphonato)dirubidium
 [Rb2(H2O){12-NH(CH2PO3H)3}]: Synthesis and Structure
;
_journal_issue                   5
_journal_name_full
;
 Crystallography Reports
;
_journal_page_first              734
_journal_page_last               738
_journal_paper_doi               10.1134/S1063774517050212
_journal_volume                  62
_journal_year                    2017
_chemical_formula_sum            'C3 H12 N O10 P3 Rb2'
_chemical_formula_weight         485.99
_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             2015-12-22T13:06:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                113.252(4)
_cell_angle_beta                 105.391(3)
_cell_angle_gamma                96.182(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0380(3)
_cell_length_b                   9.0522(4)
_cell_length_c                   10.7837(4)
_cell_measurement_reflns_used    7676
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.828
_cell_measurement_theta_min      3.743
_cell_volume                     674.77(5)
_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-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 0.997
_diffrn_measured_fraction_theta_max 0.904
_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      -0.0703049
_diffrn_orient_matrix_UB_12      -0.0411309
_diffrn_orient_matrix_UB_13      -0.0667317
_diffrn_orient_matrix_UB_21      0.0540198
_diffrn_orient_matrix_UB_22      -0.0513171
_diffrn_orient_matrix_UB_23      -0.0290305
_diffrn_orient_matrix_UB_31      -0.0320531
_diffrn_orient_matrix_UB_32      -0.0582402
_diffrn_orient_matrix_UB_33      0.0220502
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13687
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.977
_diffrn_reflns_theta_min         3.591
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.652
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41 (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    2.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.493
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.5770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0
_reflns_number_gt                4109
_reflns_number_total             4590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmpzxx9n_oe
_cod_data_source_block           rbatmp
_cod_database_code               1564825