Imidodiphosphinate ligands as antenna units in luminescent lanthanide complexes
Magennis, Steven W.; Parsons, Simon; Pikramenou, Zoe; Corval, Anne; Derek Woollins, J.; Chemical Communications  (1999) 61–; doi:10.1039/a808046a

data_7115252
_publ_section_title
;
 Imidodiphosphinate ligands as antenna units in luminescent lanthanide
 complexes
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              61
_journal_paper_doi               10.1039/a808046a
_journal_year                    1999
_chemical_formula_moiety         '[Tb(Ph2PONPOPh2)3].0.75H2O'
_chemical_formula_sum            'C72 H61.5 N3 O6.75 P6 Tb'
_chemical_formula_weight         1421.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   'geometric; disordered H not placed'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   23.372(4)
_cell_length_b                   23.372(4)
_cell_length_c                   42.956(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      11
_cell_volume                     20321(6)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_method       'Omega-theta with learnt-profile'
_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  0.1601
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9599
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.58
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'xshape vs psi-scans'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tablet developed in (001)'
_exptl_crystal_F_000             8682
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+146.1677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                5674
_reflns_number_total             7979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            808046a.txt
_cod_data_source_block           smtbp2
_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:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Numerical'
changed to 'numerical' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        20320(6)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C72 H61.50 N3 O6.75 P6 Tb'
_cod_database_code               7115252