Redox-active heterobinuclear triazenide-bridged complexes; ancillary ligand control of electron distribution in a three-electron metal‒metal bond
Connelly, Neil G.; Hayward, Owen D.; Klangsinsirikul, Phimphaka; Orpen, A. Guy; Rieger, Philip H.; Chemical Communications  (2000) 963–; doi:10.1039/b001764g

data_7110916
_publ_section_title
;
 Redox-active heterobinuclear triazenide-bridged complexes; ancillary
 ligand control of electron distribution in a three-electron metal--metal
 bond
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              963
_journal_paper_doi               10.1039/b001764g
_journal_year                    2000
_chemical_formula_sum            'C67.5 H60 Cl3 F6 Ir N6 O2 P3 Rh'
_chemical_formula_weight         1595.58
_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                97.712(12)
_cell_angle_beta                 98.499(19)
_cell_angle_gamma                90.430(12)
_cell_formula_units_Z            2
_cell_length_a                   12.967(3)
_cell_length_b                   13.714(2)
_cell_length_c                   19.830(3)
_cell_measurement_reflns_used    142
_cell_measurement_temperature    173(2)
_cell_volume                     3454.7(11)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 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      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1239
_diffrn_reflns_av_sigmaI/netI    0.1873
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29499
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.412
_exptl_absorpt_correction_T_max  0.719334
_exptl_absorpt_correction_T_min  0.422135
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick 1996'
_exptl_crystal_colour            'Dark orange'
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.125
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         12092
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                6560
_reflns_number_total             12092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001764gsup1.cif
_cod_data_source_block
4+.[Rh(CO)(PPh3)(mu-RNNNR)2Ir(CO)(PPh3)][PF6].1.5CH2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C67.50 H60 Cl3 F6 Ir N6 O2 P3 Rh'
_cod_database_code               7110916