Bi-edge condensation of imido‒rhodium clusters leading to novel planar hexametallic structures
Tejel, Cristina; Bordonaba, Marta; Ciriano, Miguel A.; Lahoz, Fernando J.; Oro, Luis A.; Chemical Communications  (1999) 2387–; doi:10.1039/a907853c

data_7110730
_publ_section_title
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 Bi-edge condensation of imido--rhodium clusters leading to novel planar
 hexametallic structures
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2387
_journal_paper_doi               10.1039/a907853c
_journal_year                    1999
_chemical_formula_moiety         'C40 H28 N4 O12 Rh6'
_chemical_formula_sum            'C40 H28 N4 O12 Rh6'
_chemical_formula_weight         1374.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1187(8)
_cell_length_b                   12.1187(8)
_cell_length_c                   29.753(3)
_cell_measurement_reflns_used    83
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4369.6(6)
_computing_cell_refinement       'XSCANS, Siemens'
_computing_data_collection       'XSCANS, Siemens SMART'
_computing_data_reduction        'SAINT program, v. 4.0 (Siemens, 1995)'
_computing_molecular_graphics    'XP, SHELXTL v. 5.0 (Siemens, 1994)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens SMART CCD Diffractometer'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.1223
_diffrn_reflns_av_sigmaI/netI    0.1663
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            15970
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.278
_exptl_absorpt_correction_T_max  0.9559
_exptl_absorpt_correction_T_min  0.8212
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'North, Phillips and Mathews, Acta Cryst. 1968, A24, 351'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       laminar
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.11(6)
_refine_ls_extinction_coef       0.00027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                3329
_reflns_number_total             5400
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            907853csup1.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4369.7(6)
_cod_database_code               7110730