New binuclear bis(2,4,6,8-tetramethyl-2,4,6,8-tetraazobicyclo(3.3.0)octane-3,7-dione-O,O')-tetraaqua-hexakis(nitrato-O,O')-disamarium(III) complex: Synthesis and crystal structure
Netreba, E.E.; Sarnit, E.A.; Shabanov, S.V.; Velikozhon, A.A.; Russian Journal of Inorganic Chemistry 62 (2017) 654–658; doi:10.1134/S0036023617050175

data_4038956
_publ_section_title
;
 New binuclear
 bis(2,4,6,8-tetramethyl-2,4,6,8-tetraazobicyclo(3.3.0)octane-3,7-dione-O,O')-tetraaqua-hexakis(nitrato-O,O')-disamarium(III)
 complex: Synthesis and crystal structure
;
_journal_issue                   5
_journal_name_full
;
 Russian Journal of Inorganic Chemistry
;
_journal_page_first              654
_journal_page_last               658
_journal_paper_doi               10.1134/S0036023617050175
_journal_volume                  62
_journal_year                    2017
_chemical_formula_sum            'C16 H36 N14 O26 Sm2'
_chemical_formula_weight         1141.29
_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             2016-02-02T12:16:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                74.475(2)
_cell_angle_beta                 67.802(2)
_cell_angle_gamma                67.570(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8661(2)
_cell_length_b                   10.2913(3)
_cell_length_c                   10.9629(3)
_cell_measurement_reflns_used    14627
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.836
_cell_measurement_theta_min      3.974
_cell_volume                     942.68(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      -0.0540239
_diffrn_orient_matrix_UB_12      -0.02196
_diffrn_orient_matrix_UB_13      0.0585711
_diffrn_orient_matrix_UB_21      -0.0186991
_diffrn_orient_matrix_UB_22      -0.0331611
_diffrn_orient_matrix_UB_23      -0.0377492
_diffrn_orient_matrix_UB_31      0.058497
_diffrn_orient_matrix_UB_32      -0.0640002
_diffrn_orient_matrix_UB_33      0.0114612
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17453
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         3.548
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.196
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.749
_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    2.01
_exptl_crystal_description       prism
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.78
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5736
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0146
_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^)+(0.0194P)^2^+0.1564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0381
_reflns_Friedel_coverage         0
_reflns_number_gt                5518
_reflns_number_total             5736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp_2ipxhyi
_cod_data_source_block           127_smmk
_cod_database_code               4038956