Crystal Structures of Lanthanide(III) Complexes with Cyclen Derivative Bearing Three Acetate and One Methylphosphonate Pendants
Pavel Vojtíšek; Petr Cígler; Jan Kotek; Jakub Rudovský; Petr Hermann; Ivan Lukeš; Inorganic Chemistry 44 (2005) 5591–5599; doi:10.1021/ic048190s

data_4309307
_publ_contact_author_address
;
Dept. of Inorganic Chemistry, Faculty of Science, Charles University
Hlavova 2030
128 40 Prague 2
Czech Republic
;
_publ_contact_author_email       pavojt@natur.cuni.cz
_publ_contact_author_name        'Vojt\'i\<sek, Pavel'
_publ_section_title
;
Crystal Structures of Lanthanide(III) Complexes with Cyclen Derivative
Bearing Three Acetate and One Methylphosphonate Pendants
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5591
_journal_page_last               5599
_journal_paper_doi               10.1021/ic048190s
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C15 H26 Lu N4 O9 P, 6(H2 O)'
_chemical_formula_sum            'C15 H38 Lu N4 O15 P'
_chemical_formula_weight         720.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.7420(10)
_cell_angle_beta                 83.3640(10)
_cell_angle_gamma                68.3550(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7320(2)
_cell_length_b                   9.3130(2)
_cell_length_c                   16.8830(4)
_cell_measurement_temperature    150(2)
_cell_volume                     1262.36(5)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23023
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.051
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.008
_refine_diff_density_min         -2.925
_refine_diff_density_rms         0.216
_refine_ls_extinction_coef       0.0054(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+6.7893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                5251
_reflns_number_total             5740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048190ssi20041222_101635_4.cif
_cod_data_source_block           lukys
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_database_code               4309307