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_4339835
_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            'C61 H60 N3 O37 Rh17'
_chemical_formula_weight         3176.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_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                 109.257(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.4555(15)
_cell_length_b                   13.8637(15)
_cell_length_c                   26.961(3)
_cell_measurement_reflns_used    4495
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      19.917
_cell_measurement_theta_min      2.535
_cell_volume                     8629.5(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0840
_diffrn_reflns_av_sigmaI/netI    0.1418
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14688
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    3.237
_exptl_absorpt_correction_T_max  0.7379
_exptl_absorpt_correction_T_min  0.5934
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             6032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.791
_refine_diff_density_min         -2.228
_refine_diff_density_rms         0.320
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         8912
_refine_ls_number_restraints     900
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.1083
_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^)+(0.0943P)^2^+344.7293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2491
_reflns_number_gt                6383
_reflns_number_total             8912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0623718-file001.cif
_cod_data_source_block           cc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        8629.7(14)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4339835