Synthesis, Isolation, and Characterization of Trisodium Tricarbonyliridate (3-), Na3[Ir(CO)3]. Initial Studies on Its Derivative Chemistry and Structural Characterizations of trans-[Ir(CO)3(EPh3)2]-, E = Ge, Sn, and trans-[Co(CO)3(SnPh3)2]-,1
Jessica M. Allen; William W. Brennessel; Carrie E. Buss; John E. Ellis; Mikhail E. Minyaev; Maren Pink; Garry F. Warnock; Mark L. Winzenburg; Victor G. Young; Inorganic Chemistry 40 (2001) 5279–5284; doi:10.1021/ic0105011

data_4320333
_publ_section_title
;
 Synthesis, Isolation, and Characterization of Trisodium
 Tricarbonyliridate (3-), Na3[Ir(CO)3]. Initial Studies on Its Derivative
 Chemistry and Structural Characterizations of trans-[Ir(CO)3(EPh3)2]-, E
 = Ge, Sn, and trans-[Co(CO)3(SnPh3)2]-,1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5279
_journal_page_last               5284
_journal_paper_doi               10.1021/ic0105011
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C39 H30 Ge2 Ir O3, C8 H20 N, C H2 Cl2'
_chemical_formula_sum            'C48 H52 Cl2 Ge2 Ir N O3'
_chemical_formula_weight         1099.19
_chemical_name_common            00172
_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                 106.946(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.722(3)
_cell_length_b                   9.7797(11)
_cell_length_c                   20.679(2)
_cell_measurement_reflns_used    4978
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.252
_cell_measurement_theta_min      2.304
_cell_volume                     4589.1(9)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20663
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    4.351
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.748451
_exptl_absorpt_correction_type   multiscans
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.548
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9783
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                8993
_reflns_number_total             9783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0105011_2.cif
_cod_data_source_block           00172
_cod_original_cell_volume        4589.2(9)
_cod_database_code               4320333