Skeletal Growth by Condensation of Small Metal Fragments on a Carbido Carbonyl Cluster. Synthesis of the Anions [Rh15C2(CO)24X2]3-(X = Cl, Br, I) and Molecular Structure of the Bromo and Iodo Derivatives
Fumagalli, Alessandro; Martinengo, Secondo; Bernasconi, Giovanni; Noziglia, Luciana; Albano, Vincenzo G.; Monari, Magda; Castellari, Carlo; Organometallics 19 (2000) 5149–; doi:10.1021/om000577p

data_4077608
_publ_section_title
;
 Skeletal Growth by Condensation of Small Metal Fragments on a Carbido
 Carbonyl Cluster. Synthesis of the Anions [Rh15C2(CO)24X2]3-(X = Cl, Br,
 I) and Molecular Structure of the Bromo and Iodo Derivatives
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5149
_journal_paper_doi               10.1021/om000577p
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C50.9 H60.3 I2 N3 O24.81 Rh15'
_chemical_formula_weight         2908.61
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8365(2)
_cell_length_b                   15.0577(2)
_cell_length_c                   24.9047(3)
_cell_measurement_temperature    293(2)
_cell_volume                     7797.62(16)
_computing_cell_refinement       'SMART-NT V5.0 (Bruker 1998)'
_computing_data_collection       'SMART-NT V5.0 (Bruker 1998)'
_computing_data_reduction        'SAINT-NT V5.0 (Bruker 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART-CCD'
_diffrn_measurement_method       /w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17662
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.940
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.478
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             5465
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.988
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     749
_refine_ls_number_reflns         17654
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.011
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_obs          0.0269
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0694
_refine_ls_wR_factor_obs         0.0648
_reflns_number_observed          13507
_reflns_number_total             17662
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om000577p.cif
_cod_data_source_block           rhir
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0378P)^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^)+(0.0378P)^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        7797.6(2)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C50.90 H60.30 I2 N3 O24.81 Rh15'
_cod_database_code               4077608