Synthesis and characterisation of dimeric eight-coordinate lanthanide(III) complexes of a macrocyclic tribenzylphosphinate ligand.
Senanayake, Kanthi; Thompson, Amber L.; Howard, Judith A. K.; Botta, Mauro; Parker, David; Dalton transactions (Cambridge, England : 2003)  (2006) 5423–5428; doi:10.1039/b612189f

data_7007881
_publ_section_title
;
 Synthesis and characterisation of dimeric eight-coordinate
 lanthanide(III) complexes of a macrocyclic tribenzylphosphinate
 ligand.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5423
_journal_page_last               5428
_journal_paper_doi               10.1039/b612189f
_journal_year                    2006
_chemical_formula_moiety         'C64 H88 Gd2 N8 O12 P6, 10(O H2)'
_chemical_formula_sum            'C64 H108 Gd2 N8 O22 P6'
_chemical_formula_weight         1841.90
_chemical_melting_point          ?
_chemical_name_common
;
bis((mu!2$-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl-
methyl-(trimethylene-tris(phenylphosphinato)))-gadolinium(iii))
decahydrate
;
_chemical_name_systematic
;
bis((\m~2~-1-4-7-10-tetra-azacyclododecane-1,4,7,10-tetrayl-methyl-
(trimethylene-tris(phenylphosphinato)))-gadolinium(III)) decahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.0290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6618(7)
_cell_length_b                   15.1330(6)
_cell_length_c                   30.2751(13)
_cell_measurement_reflns_used    9348
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.462
_cell_measurement_theta_min      2.361
_cell_volume                     7576.3(5)
_computing_cell_refinement       'SMART-NT V6.1 (Bruker, 2000)'
_computing_data_collection       'SMART-NT V6.1 (Bruker, 2000)'
_computing_data_reduction        'SAINT-NT V6.45A (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       \w-scans
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            31846
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.9621
_exptl_absorpt_correction_T_min  0.7693
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (SHELXTL,1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8657
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0473
_reflns_number_gt                6503
_reflns_number_total             8657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b612189f.txt
_cod_data_source_block           '[Gd.L^3^]~2~.10H~2~O'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Integration' changed
to 'integration' according to
'/home/adriana/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7007881