Crystal structure of a new binuclear complex of bis(2,4,6,8-tetramethyl-2,4,6,8-tetraazabicyclo(3.3.0)octane -3,7-dione-O, O)-diaqua-hexakis(nitrato-O,O)-digadolinium(III) monohydrate
Netreba, E.E.; Somov, N.V.; Journal of Structural Chemistry 58 (2017) 838–842; doi:10.1134/S0022476617040321

data_1564824
_publ_section_title
;
 Crystal structure of a new binuclear complex of
 bis(2,4,6,8-tetramethyl-2,4,6,8-tetraazabicyclo(3.3.0)octane
 -3,7-dione-O, O)-diaqua-hexakis(nitrato-O,O)-digadolinium(III)
 monohydrate
;
_journal_issue                   4
_journal_name_full
;
 Journal of Structural Chemistry
;
_journal_page_first              838
_journal_page_last               842
_journal_paper_doi               10.1134/S0022476617040321
_journal_volume                  58
_journal_year                    2017
_chemical_formula_sum            'C16 H36 Gd2 N14 O26'
_chemical_formula_weight         1155.09
_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             2016-01-28T12:58:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 128.413(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3861(2)
_cell_length_b                   10.80470(10)
_cell_length_c                   21.2707(4)
_cell_measurement_reflns_used    21715
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.864
_cell_measurement_theta_min      3.677
_cell_volume                     1870.32(8)
_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 0.927
_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      -0.0761489
_diffrn_orient_matrix_UB_12      0.0317261
_diffrn_orient_matrix_UB_13      -0.0249958
_diffrn_orient_matrix_UB_21      -0.0297004
_diffrn_orient_matrix_UB_22      -0.0344644
_diffrn_orient_matrix_UB_23      0.0169927
_diffrn_orient_matrix_UB_31      0.030251
_diffrn_orient_matrix_UB_32      0.0459901
_diffrn_orient_matrix_UB_33      0.0299708
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36780
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.052
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.628
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.59187
_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    2.051
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.27
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.019
_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^)+(0.0122P)^2^+1.2876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0
_reflns_number_gt                6269
_reflns_number_total             6565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tmp2mlw6qi7
_cod_data_source_block           122_gdmk
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564824