Synthesis, Solid-State Structure and Solution Behavior of Hydrido-Bridged Adducts between the Group 11 [M(PPh3)]+Cations and the Triangular Cluster Anion [Re3(μ-H)4(CO)9(PPh3)]-
Beringhelli, Tiziana; D'Alfonso, Giuseppe; Garavaglia, Maria Grazia; Panigati, Monica; Mercandelli, Pierluigi; Sironi, Angelo; Organometallics 21 (2002) 2705–; doi:10.1021/om0200252

data_4076787
_publ_section_title
;
 Synthesis, Solid-State Structure and Solution Behavior of Hydrido-Bridged
 Adducts between the Group 11 [M(PPh3)]+Cations and the Triangular Cluster
 Anion [Re3(\m-H)4(CO)9(PPh3)]-
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2705
_journal_paper_doi               10.1021/om0200252
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C45 H34 Cu O9 P2 Re3'
_chemical_formula_sum            'C45 H34 Cu O9 P2 Re3'
_chemical_formula_weight         1402.80
_chemical_melting_point          ?
_chemical_name_systematic
;
 nonacarbonyltri-\m-hydrido-\m~3~-hydrido(triphenylphosphine)
 [(triphenylphosphine)copper]trirhenium
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.91(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.317(5)
_cell_length_b                   28.035(9)
_cell_length_c                   17.556(7)
_cell_measurement_reflns_used    16958
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.32
_cell_volume                     4552(3)
_computing_structure_refinement
;
 Sheldrick, G. M. SHELX97: program for crystal structure refinement;
 University of G\"ottingen: G\"ottingen, 1996.
;
_computing_structure_solution
;
 SIR97: Altomare, A.; Burla, M. C.; Camalli, M.; Cascarano, G. L.;
 Giacovazzo, C.; Guagliardi, A.; Moliterni, A. G. G.; Polidori, G.;
 Spagna, R. J. Appl. Crystallogr. 1999, 32, 115.
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 Unit cell parameters were initially obtained from 100 reflections
 (5\% < \q < 20\%) taken from 45 frames collected in three different
 \w regions.
 A full sphere of reciprocal space was scanned by 0.3\% \w steps,
 collecting 1800 frames each at 40 s exposure.
 The detector was kept at 3.88(2) cm from the sample.
 Intensity decay was monitored by recollecting the initial 100 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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39297
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.535
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Sheldrick, G. M. SADABS: program for empirical absorption correction;
 University of G\"ottingen: G\"ottingen, 1996.
 28597 symmetry equivalent reflection intensities.
 Average redundancy: 4.84.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8032
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                6819
_reflns_number_total             8032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om0200252.cif
_cod_data_source_block           4-monoclinic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076787