A heteropentanuclear oxalato-bridged [ReIV4GdIII] complex: synthesis, crystal structure and magnetic properties Attachment c.- Revised_CIF
Jose Martinez-Lillo; Laura Canadillas-Delgado; Joan Cano; Francesc Lloret; Miguel Julve; J.Faus; Chem.Commun. 48 (2012) 9242–; doi:10.1039/c2cc33350c

data_7108316
_publ_section_title
;
 A heteropentanuclear oxalato-bridged [ReIV4GdIII] complex: synthesis,
 crystal structure and magnetic properties Attachment c.- Revised_CIF
;
_journal_name_full               Chem.Commun.
_journal_page_first              9242
_journal_paper_doi               10.1039/c2cc33350c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C88 H184 Br16 Gd N5 O18 Re4'
_chemical_formula_weight         3781.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 91.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.171(4)
_cell_length_b                   27.492(6)
_cell_length_c                   27.062(5)
_cell_measurement_reflns_used    130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.4
_cell_volume                     13514(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'mxcube (Gabadinho & McSweeney, 2010'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXH-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'HUBER ADSC Q210r CCD detector'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.73800
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58915
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.40
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    8.836
_exptl_absorpt_correction_T_max  0.5383
_exptl_absorpt_correction_T_min  0.4719
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
before sphere absorption correction
_diffrn_reflns_av_R_equivalents 0.0855
_diffrn_reflns_av_sigmaI/netI 0.1007
after sphere absorption correction
_diffrn_reflns_av_R_equivalents 0.0851
_diffrn_reflns_av_sigmaI/netI 0.1002
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7260
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.909
_refine_diff_density_min         -2.747
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         28250
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+98.3948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                25775
_reflns_number_total             28250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc33350c.txt
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7108316