Structural characterisation of a diprotonated ligand lanthanide complex‒a key intermediate in lanthanide ion association and complex dissociation pathways.
Stenson, Philip A.; Thompson, Amber L.; Parker, David; Dalton transactions (Cambridge, England : 2003)  (2006) 3291–3293; doi:10.1039/b605876k

data_7007466
_publ_section_title
;
 Structural characterisation of a diprotonated ligand lanthanide
 complex--a key intermediate in lanthanide ion association and complex
 dissociation pathways.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3291
_journal_page_last               3293
_journal_paper_doi               10.1039/b605876k
_journal_year                    2006
_chemical_formula_moiety         'C16 H42 Gd N8 O8, 5(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C16 H48 Cl5 Gd N8 O31'
_chemical_formula_weight         1183.12
_chemical_melting_point          ?
_chemical_name_common
;
Tetra-aqua-(1,4,7,10-terakis(carbamoylmethyl)-1,7-diaza-4,10-
diazoniumcyclodecane)-gadolinium penta-perchlorate trihydrate
;
_chemical_name_systematic
;
Tetra-aqua-(1,4,7,10-terakis(carbamoylmethyl)-
1,7-diaza-4,10-diazoniumcyclodecane)-gadolinium
penta-perchlorate trihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.0440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2765(5)
_cell_length_b                   18.3391(7)
_cell_length_c                   19.7210(8)
_cell_measurement_reflns_used    7865
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.077
_cell_measurement_theta_min      2.350
_cell_volume                     4068.2(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47754
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  0.8854
_exptl_absorpt_correction_T_min  0.6733
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (SHELXTL,1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         10883
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0280P)^2^+8.4630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                9166
_reflns_number_total             10883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605876k.txt
_cod_data_source_block           3
_cod_depositor_comments
;
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      P2(1)/n
_cod_database_code               7007466