Synthesis and electrochemistry of new Rh-centered and conjuncto rhodium carbonyl clusters. X-ray structure of [NEt(4)](3)[Rh(15)(CO)(27)], [NEt(4)](3)[Rh(15)(CO)(25)(MeCN)(2)] x 2MeCN, and [NEt(4)](3)[Rh(17)(CO)(37)].
Collini, Davide; Biani, Fabrizia Fabrizi De; Fedi, Serena; Femoni, Cristina; Kaswalder, Francesco; Iapalucci, Maria Carmela; Longoni, Giuliano; Tiozzo, Cristina; Zacchini, Stefano; Zanello, Piero; Inorganic chemistry 46 (2007) 7971–7981; doi:10.1021/ic0623718

data_4339833
_publ_section_title
;
 Synthesis and electrochemistry of new Rh-centered and conjuncto rhodium
 carbonyl clusters. X-ray structure of [NEt(4)](3)[Rh(15)(CO)(27)],
 [NEt(4)](3)[Rh(15)(CO)(25)(MeCN)(2)] x 2MeCN, and
 [NEt(4)](3)[Rh(17)(CO)(37)].
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7971
_journal_page_last               7981
_journal_paper_doi               10.1021/ic0623718
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C51 H60 N3 O27 Rh15'
_chemical_formula_weight         2690.67
_chemical_name_systematic
; 
 ? 
;
_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                88.282(2)
_cell_angle_beta                 88.360(2)
_cell_angle_gamma                88.004(2)
_cell_formula_units_Z            4
_cell_length_a                   16.867(2)
_cell_length_b                   18.898(3)
_cell_length_c                   23.275(3)
_cell_measurement_reflns_used    7100
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.044
_cell_measurement_theta_min      2.319
_cell_volume                     7408.3(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70757
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    3.316
_exptl_absorpt_correction_T_max  0.7773
_exptl_absorpt_correction_T_min  0.6361
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.523
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1766
_refine_ls_number_reflns         26008
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0993P)^2^+99.6408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                16160
_reflns_number_total             26008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0623718-file001.cif
_cod_data_source_block           p-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        7408.4(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339833