A Methyl Group Bridging on Three Metal Atoms. Solid-State and Solution Structural Characterization of the [Re3(μ-H)3(μ3-CH3)(CO)9]- Anion
T. Beringhelli; G. D'Alfonso; M. Panigati; F. Porta; P. Mercandelli; M. Moret; A. Sironi; Journal of the American Chemical Society 121 (1999) 2307–2308; doi:10.1021/ja983379m

data_4116309
_publ_section_title
;
 A Methyl Group Bridging on Three Metal Atoms. Solid-State and Solution
 Structural Characterization of the [Re3(\m-H)3(\m3-CH3)(CO)9]- Anion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2307
_journal_page_last               2308
_journal_paper_doi               10.1021/ja983379m
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C24 H20 P 1+, C10 H6 O9 Re3 1-, C4 H10 O'
_chemical_formula_sum            'C38 H36 O10 P Re3'
_chemical_formula_weight         1242.24
_chemical_name_systematic
;
 tetraphenylphosphonium nonacarbonyltri(\m-hydrido)(\m~3~-methyl)trirhenate
 diethylether solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.36(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.083(3)
_cell_length_b                   12.329(1)
_cell_length_c                   23.834(3)
_cell_measurement_reflns_used    6809
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     4104.2(11)
_computing_structure_refinement
;
 Sheldrick, G. M. SHELX-97: program for crystal structure refinement;
 University of Go\"ttingen: Go\"ttingen, 1996.
;
_computing_structure_solution
;
 SIR96: Altomare, A.; Cascarano, G.; Giacovazzo, C.; Guagliardi, A.;
 Burla, M. C.; Polidori, C.; Camalli, M. J. Appl. Crystallogr. 1994, 27,=
 435.
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details
;
 Unit cell parameters were initially obtained from 234 reflections
 (5 < \q < 21) taken from 45 frames collected in three different \w regions.
 A full sphere of reciprocal space was scanned by 0.3=B0 \w steps,
 collecting 2500 frames each at 20 s exposure.
 The detector was kept at 5.50(2) cm from the sample.
 Intensity decay was monitored by recollecting the initial 50 frames
 at the end of data collection and analyzing the duplicate reflections.
;
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44840
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.917
_exptl_absorpt_correction_T_max  0.1020
_exptl_absorpt_correction_T_min  0.0427
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Sheldrick, G. M. SADABS: program for empirical absorption correction;
 University of Go\"ttingen: Go\"ttingen, 1996.
 32429 symmetry equivalent reflection intensities.
 Average redundancy: 4.70
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       cube
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0220P)^2^] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0463
_refine_ls_wR_factor_gt          0.0443
_reflns_number_gt                6989
_reflns_number_total             9356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja983379m.cif
_cod_data_source_block           monica5
_cod_database_code               4116309