Synthesis, crystal structures and NMR and luminescence spectra of lanthanide complexes of 1,4,7,10-tetraazacyclododecane with N-methylene(phenyl)phosphinic acid pendant arms †
Rohovec, Jan; Vojtíšek, Pavel; Hermann, Petr; Mosinger, Jiří; Žák, Zdirad; Lukeš, Ivan; Journal of the Chemical Society, Dalton Transactions  (1999) 3585–; doi:10.1039/a905460j

data_7027676
_publ_section_title
;
 Synthesis, crystal structures and NMR and luminescence spectra of
 lanthanide complexes of 1,4,7,10-tetraazacyclododecane with
 N-methylene(phenyl)phosphinic acid pendant arms&#x200A;&#x2020;
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_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3585
_journal_paper_doi               10.1039/a905460j
_journal_year                    1999
_chemical_formula_moiety         Li[La(H2O)(C8H16N4(CH2P(C6H5)O2)4)]*10H2O
_chemical_formula_sum            'C36 H66 La Li N4 O19 P4'
_chemical_formula_weight         1128.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson, Fourier '
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.855(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.145(2)
_cell_length_b                   24.4580(10)
_cell_length_c                   20.160(2)
_cell_measurement_reflns_used    4926
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      1.8
_cell_volume                     10888.2(17)
_computing_cell_refinement       'KUMA  (Poland)'
_computing_data_collection       'KUMA  (Poland)'
_computing_data_reduction        'KUMA  (Poland)'
_computing_molecular_graphics    'PLATON-92 (Spek, 1992)'
_computing_publication_material  WORD
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(1)
_diffrn_detector_area_resol_mean '16.7 pixels/mm'
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'KUMA (Poland)'
_diffrn_measurement_method       '.omega.-scan (0.5.degree) '
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            86193
_diffrn_reflns_theta_full        28.60
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        --
_diffrn_standards_interval_count --
_diffrn_standards_interval_time  --
_diffrn_standards_number         --
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  --
_exptl_absorpt_correction_T_min  --
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.662
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       --
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.546
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1205
_refine_ls_number_reflns         25133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.546
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.1239
_refine_ls_shift/su_max          4.609
_refine_ls_shift/su_mean         0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3412
_refine_ls_wR_factor_ref         0.3942
_reflns_number_gt                17475
_reflns_number_total             25133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905460Jsup1.cif
_cod_data_source_block           laend21
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '--' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        10888.2(15)
_cod_original_sg_symbol_H-M      'P2(1)/c  (no. 14)'
_cod_database_code               7027676