Stoichiometry of lanthanide(iii) complexes with tripodal aminophosphonic ligands ‒ a new solution to an old problem
Janicki, Rafał; Gałęzowska, Joanna; Mondry, Anna; Inorganic Chemistry Frontiers 4 (2017) 1200–; doi:10.1039/C7QI00191F

data_4349706
_publ_section_title
;
 Stoichiometry of lanthanide(iii) complexes with tripodal aminophosphonic
 ligands -- a new solution to an old problem
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1200
_journal_paper_doi               10.1039/C7QI00191F
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C21 H74 Gd N19 O24 P4'
_chemical_formula_weight         1258.12
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-04-03 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                105.710(5)
_cell_angle_beta                 94.360(4)
_cell_angle_gamma                90.901(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9496(6)
_cell_length_b                   14.1528(7)
_cell_length_c                   16.1651(9)
_cell_measurement_reflns_used    2320
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5185
_cell_measurement_theta_min      2.7137
_cell_volume                     2622.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.9814
_diffrn_measured_fraction_theta_max 0.9871
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_sigmaI/netI    0.2448
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23976
_diffrn_reflns_theta_full        29.5096
_diffrn_reflns_theta_max         31.59
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   'analytical, from the shape'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1298
_exptl_crystal_size_max          0.2712
_exptl_crystal_size_mid          0.0522
_exptl_crystal_size_min          0.0153
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         15463
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.1014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                8529
_reflns_number_total             15463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qi00191f2.cif
_cod_data_source_block           gdnp2pya
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4349706