Derivative of cyclen with three methylene(phenyl)phosphinic acid pendant arms. Synthesis and crystal structures of its lanthanide complexes
Rohovec, Jan; Vojtíšek, Pavel; Hermann, Petr; Ludvík, Jiří; Lukeš, Ivan; Journal of the Chemical Society, Dalton Transactions  (2000) 141–; doi:10.1039/a907018d

data_7008923
_publ_section_title
;
 Derivative of cyclen with three methylene(phenyl)phosphinic acid
 pendant arms. Synthesis and crystal structures of its lanthanide
 complexes
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              141
_journal_paper_doi               10.1039/a907018d
_journal_year                    2000
_chemical_formula_moiety         '[Ce(H2O)L]2*8H2O*2MeOH '
_chemical_formula_sum            'C32 H60 Ce N4 O13 P3'
_chemical_formula_weight         941.87
_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                 107.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.194(3)
_cell_length_b                   19.990(4)
_cell_length_c                   15.534(3)
_cell_measurement_reflns_used    4926
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      1.8
_cell_volume                     3913.6(15)
_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      170(1)
_diffrn_detector_area_resol_mean '16.7 pixels/mm  '
_diffrn_measured_fraction_theta_full 0.790
_diffrn_measured_fraction_theta_max 0.790
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28519
_diffrn_reflns_theta_full        30.67
_diffrn_reflns_theta_max         30.67
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        --
_diffrn_standards_interval_count --
_diffrn_standards_interval_time  --
_diffrn_standards_number         --
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  --
_exptl_absorpt_correction_T_min  --
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         4.514
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.297
_refine_ls_extinction_coef       0.0029(4)
_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   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         9815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          9.527
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+17.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                7669
_reflns_number_total             9815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907018d.txt
_cod_data_source_block           ct13e
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+17.4923P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1031P)^2^+17.4923P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3913.6(14)
_cod_original_sg_symbol_H-M      'P2(1)/c  (no. 14)'
_cod_database_code               7008923