Large Effects of Ion Pairing and Protonic-Hydridic Bonding on the Stereochemistry and Basicity of Crown-, Azacrown-, and Cryptand-222-potassium Salts of Anionic Tetrahydride Complexes of Iridium(III)
Shaun E. Landau; Kai E. Groh; Alan J. Lough; Robert H. Morris; Inorganic Chemistry 41 (2002) 2995–3007; doi:10.1021/ic0255149

data_4318052
_publ_section_title
;
 Large Effects of Ion Pairing and Protonic-Hydridic Bonding on the
 Stereochemistry and Basicity of Crown-, Azacrown-, and
 Cryptand-222-potassium Salts of Anionic Tetrahydride Complexes of
 Iridium(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2995
_journal_page_last               3007
_journal_paper_doi               10.1021/ic0255149
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C54 H74 Ir K N2 O5.5 P2'
_chemical_formula_weight         1132.39
_chemical_name_common            '[K(diaza-18-crown-6)][IrH4(PPh3)2]'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 121.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.056(7)
_cell_length_b                   14.394(3)
_cell_length_c                   23.799(5)
_cell_measurement_temperature    150.0(1)
_cell_volume                     10575(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD server software (Nonius, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.064
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            39781
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    2.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN, (Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.429
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.000083(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         10633
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+35.3854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                8846
_reflns_number_total             10633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255149_s1_2.cif
_cod_data_source_block           kdiaza5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        10575(4)
_cod_original_formula_sum        'C54 H74 Ir K N2 O5.50 P2'
_cod_database_code               4318052