Fixation and spontaneous dehydrogenation of methanol on a triruthenium‒iridium framework: synthesis and structure of the cluster anion [HRu3Ir(CO)12(OMe)]−
Haak, Susanne; Neels, Antonia; Stœckli-Evans, Helen; Süss-Fink, Georg; Thomas, Christophe M.; Chemical Communications  (1999) 1959–; doi:10.1039/a905487a

data_7110647
_publ_section_title
;
 Fixation and spontaneous dehydrogenation of methanol on a
 triruthenium--iridium framework: synthesis and structure of the cluster
 anion [HRu3Ir(CO)12(OMe)]&#x2212;
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1959
_journal_paper_doi               10.1039/a905487a
_journal_year                    1999
_chemical_formula_sum            'C97 H66 Ir2 N2 O25 P4 Ru6'
_chemical_formula_weight         2774.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.541(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.9660(14)
_cell_length_b                   19.7432(10)
_cell_length_c                   17.0768(13)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     4989.8(7)
_computing_cell_refinement       'CELL, Stoe & Cie Company, Germany'
_computing_data_collection       'EXPOSE, Stoe & Cie Company, Germany'
_computing_data_reduction        'INTEGRATE, Stoe & Cie Company,Germany'
_computing_molecular_graphics    'PLATON97 (Spek, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'IPDS, Stoe & Cie Company, Germany'
_diffrn_measurement_method       'Phi oscillation 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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38776
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.675
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   difabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.108
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         9673
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                5302
_reflns_number_total             9673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905487asup1.cif
_cod_data_source_block           compound2and3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1056P)^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^)+(0.1056P)^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_sg_symbol_H-M      'P 21/c'
_cod_database_code               7110647