Crystal structure determination of 4f‒5f heterometallic complexes
Pascal C. Leverd; David Rinaldo; Martine Nierlich; J. Chem. Soc., Dalton Trans.  (2002) 829–831; doi:10.1039/b200199n

data_7011462
_publ_section_title
;
 Crystal structure determination of 4f--5f heterometallic complexes
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              829
_journal_page_last               831
_journal_paper_doi               10.1039/b200199n
_journal_year                    2002
_chemical_formula_sum            'C267 H295 Cl4 La2 N27 O12 U'
_chemical_formula_weight         4731.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.79(3)
_cell_angle_beta                 79.67(3)
_cell_angle_gamma                87.41(3)
_cell_formula_units_Z            1
_cell_length_a                   15.646(3)
_cell_length_b                   16.759(3)
_cell_length_c                   23.203(5)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.95
_cell_volume                     5979(2)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL, V.5, Madison/WI, 1997'
_computing_publication_material  'Bruker SHELXTL, V.5, Madison/WI, 1997'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.760
_diffrn_measured_fraction_theta_max 0.760
_diffrn_measurement_device_type  'nonius CCD'
_diffrn_measurement_method       'Phi scan'
_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  0.133
_diffrn_reflns_av_sigmaI/netI    0.2669
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26187
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         17157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.2730
_refine_ls_R_factor_gt           0.1168
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.1114P)^2^+28.8427P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.3055
_reflns_number_gt                7013
_reflns_number_total             17157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200199n.txt
_cod_data_source_block           struc
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011462