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_7008920
_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         ' [NdL]2*14H2O (!centrosymmetric dimer!) '
_chemical_formula_sum            'C30 H54 N4 Nd O13 P3'
_chemical_formula_weight         915.92
_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                 109.38(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.112(3)
_cell_length_b                   19.758(5)
_cell_length_c                   15.928(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      13
_cell_volume                     3892.6(19)
_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      170(1)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  ' CAD4  (Enraf-Nonius) '
_diffrn_measurement_method       '.omega.-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  0.0767
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5670
_diffrn_reflns_theta_full        23.01
_diffrn_reflns_theta_max         23.01
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        5.4
_diffrn_standards_interval_time  '60 min '
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_T_max  --
_exptl_absorpt_correction_T_min  --
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            'pale pink '
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.911
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.00000(19)
_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   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          5.249
_refine_ls_shift/su_mean         0.053
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+22.3266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                4286
_reflns_number_total             5405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907018d.txt
_cod_data_source_block           nd16e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+22.3266P] 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^)+(0.0960P)^2^+22.3266P] 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        3892.5(18)
_cod_original_sg_symbol_H-M      'P2(1)/c  (no. 14) '
_cod_database_code               7008920