dppm and hydrido-bridged dinuclear complexes of iridium. Synthesis and structures of [(IrCp*)2(μ-dppm)(μ-H)(μ-X)]2+ (X = Cl, OMe, OH, or H)
Fujita, Ken-ichi; Hamada, Taro; Yamaguchi, Ryohei; Journal of the Chemical Society, Dalton Transactions  (2000) 1931–; doi:10.1039/b001239o

data_7009462
_publ_section_title
;
 dppm and hydrido-bridged dinuclear complexes of iridium. Synthesis and
 structures of [(IrCp*)2(\m-dppm)(\m-H)(\m-X)]2+ (X&#x2005;=&#x2005;Cl,
 OMe, OH, or H)
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1931
_journal_paper_doi               10.1039/b001239o
_journal_year                    2000
_chemical_formula_sum            'C94 H96 B2 Ir2 O P2'
_chemical_formula_weight         1709.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 107.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.481(9)
_cell_length_b                   11.13(1)
_cell_length_c                   27.771(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291.2
_cell_measurement_theta_max      12.7
_cell_measurement_theta_min      10.6
_cell_volume                     7786(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;
'DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      291.2
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.01492
_diffrn_orient_matrix_UB_12      0.07154
_diffrn_orient_matrix_UB_13      0.01268
_diffrn_orient_matrix_UB_21      -0.03121
_diffrn_orient_matrix_UB_22      -0.00028
_diffrn_orient_matrix_UB_23      -0.03143
_diffrn_orient_matrix_UB_31      -0.01948
_diffrn_orient_matrix_UB_32      -0.05433
_diffrn_orient_matrix_UB_33      0.01686
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.04480
_diffrn_reflns_av_sigmaI/netI    0.134
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            19124
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        -3.55
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.513
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3448.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.277
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     910
_refine_ls_number_reflns         8238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0370
_refine_ls_wR_factor_ref         0.0370
_reflns_number_gt                8238
_reflns_number_total             18730
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b001239o.txt
_cod_data_source_block           '_6b'
_cod_original_cell_volume        7788(7)
_cod_original_sg_symbol_H-M      'P 21/a     '
_cod_original_formula_sum        'C94 H96 B2 Ir2 O P2 '
_cod_database_code               7009462