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_7008918
_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
'[La(H2O)L]2*10H2O (!centrosymmetric dimer!) '
_chemical_formula_sum            'C30 H52 La N4 O12 P3'
_chemical_formula_weight         892.58
_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                 108.221(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2355(12)
_cell_length_b                   20.229(4)
_cell_length_c                   15.6591(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      13
_cell_volume                     3982.4(10)
_computing_cell_refinement       'CAD4 program packet'
_computing_data_collection       'CAD4 program packet'
_computing_data_reduction        'JANA-98 (Petricek, 1998)'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'CAD4  (Enraf-Nonius) '
_diffrn_measurement_method       '.omege.-2.theta. '
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6270
_diffrn_reflns_theta_full        24.09
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        7.8
_diffrn_standards_interval_time  '60 min '
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  --
_exptl_absorpt_correction_T_min  --
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.087
_refine_diff_density_min         -2.328
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00060(18)
_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   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          9.846
_refine_ls_shift/su_mean         0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+15.4985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                5496
_reflns_number_total             6254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907018d.txt
_cod_data_source_block           la4e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+15.4985P] 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^)+(0.0827P)^2^+15.4985P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P2(1)/c  (no. 14)'
_cod_database_code               7008918