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_7027675
_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[Ce(H2O)(C8H16N4(CH2P(C6H5)O2)4)]*10H2O
_chemical_formula_sum            'C36 H66 Ce Li N4 O19 P4'
_chemical_formula_weight         1129.87
_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                 113.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.188(5)
_cell_length_b                   24.412(5)
_cell_length_c                   20.087(4)
_cell_measurement_reflns_used    5534
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      19.1
_cell_measurement_theta_min      2.1
_cell_volume                     10851(5)
_computing_cell_refinement       'KUMA program packet'
_computing_data_collection       'KUMA program packet'
_computing_data_reduction        'KUMA program packet'
_computing_molecular_graphics    'PLATON-92 (Spek, 1992)'
_computing_publication_material  WORD
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '16.7 pixels/mm '
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            85745
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.39
_diffrn_standards_decay_%        --
_diffrn_standards_interval_count --
_diffrn_standards_interval_time  --
_diffrn_standards_number         --
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  --
_exptl_absorpt_correction_T_min  --
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4664
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.631
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.719
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         25206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.719
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.1395
_refine_ls_shift/su_max          3.428
_refine_ls_shift/su_mean         0.023
_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          0.3719
_refine_ls_wR_factor_ref         0.4262
_reflns_number_gt                17356
_reflns_number_total             25206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905460Jsup1.cif
_cod_data_source_block           ceend16
_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        10851(4)
_cod_original_sg_symbol_H-M      'P2(1)/c  (no. 14)'
_cod_database_code               7027675