[Rh28N4(CO)41Hx]4-, a Massive Carbonyl Cluster with Four Interstitial Nitrogen Atoms
Alessandro Fumagalli; Secondo Martinengo; Giovanni Bernasconi; Gianfranco Ciani; Davide M. Proserpio; Angelo Sironi; Journal of the American Chemical Society 119 (1997) 1450–1451; doi:10.1021/ja961403v

data_4116932
_publ_contact_author             'Angelo Sironi'
_publ_contact_author_email       angelo@mail.csmtbo.mi.cnr.it
_publ_section_title
;
 [Rh28N4(CO)41Hx]4-, a Massive Carbonyl Cluster with Four Interstitial
 Nitrogen Atoms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1450
_journal_page_last               1451
_journal_paper_doi               10.1021/ja961403v
_journal_volume                  119
_journal_year                    1997
_chemical_formula_structural     '[Rh28N4(CO)41][N(C2H5)4]4.(CH3)2CO'
_chemical_formula_sum            'C76 H86 N8 O42 Rh28'
_chemical_formula_weight         4665.01
_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
_cell_angle_alpha                85.700(10)
_cell_angle_beta                 86.190(10)
_cell_angle_gamma                69.340(10)
_cell_formula_units_Z            2
_cell_length_a                   14.7660(10)
_cell_length_b                   16.287(2)
_cell_length_c                   25.284(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     5668.4(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       omega
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19845
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3
_diffrn_standards_decay_%        15
_diffrn_standards_interval_time  2h
_exptl_absorpt_coefficient_mu    4.028
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.733
_exptl_crystal_F_000             4388
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    riding-model
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1367
_refine_ls_number_reflns         15679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_obs          0.0286
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+(0.0374P)^2^+10.7536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0685
_reflns_number_observed          15679
_reflns_number_total             19841
_reflns_observed_criterion       >1sigma(I)
_cod_data_source_file            ja961403v.cif
_cod_data_source_block           rh28
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[s^2^(Fo^2^)+(0.0374P)^2^+10.7536P] 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^)+(0.0374P)^2^+10.7536P] 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        5668.4(9)
_cod_database_code               4116932
_exptl_absorpt_correction_nazim  3
_diffrn_measurement_domega       1.1+0.35tg(theta)
_diffrn_measurement_rtime        70