Macropolyhedral boron-containing cluster chemistry. Ligand-induced two-electron variations of intercluster bonding intimacy. Structures of nineteen-vertex [(eta5-C5Me5)HIrB18H19(PMe2Ph)] and the related carbene complex [(eta5-C5Me5)HIrB18H19[C(NHMe)2]].
Shea, Suzanne L.; Jelínek, Tomás; Perera, Sarath D.; Stíbr, Bohumil; Thornton-Pett, Mark; Kennedy, John D.; Dalton transactions (Cambridge, England : 2003)  (2004) 1521–1523; doi:10.1039/b404322g

data_7014233
_publ_section_title
;
 Macropolyhedral boron-containing cluster chemistry. Ligand-induced
 two-electron variations of intercluster bonding intimacy. Structures
 of nineteen-vertex [(eta5-C5Me5)HIrB18H19(PMe2Ph)] and the related
 carbene complex [(eta5-C5Me5)HIrB18H19[C(NHMe)2]].
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1521
_journal_page_last               1523
_journal_paper_doi               10.1039/b404322g
_journal_year                    2004
_chemical_formula_sum            'C18 H46 B18 Ir P'
_chemical_formula_weight         680.30
_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_date             98-04-09
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                99.201(8)
_cell_angle_beta                 98.006(9)
_cell_angle_gamma                90.678(8)
_cell_formula_units_Z            4
_cell_length_a                   10.2788(9)
_cell_length_b                   17.2512(15)
_cell_length_c                   18.1263(17)
_cell_measurement_reflns_used    72
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      17.5
_cell_volume                     3140.0(5)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.812
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
Scan width (omega) = 1.45 - 1.60, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10075
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.314
_exptl_absorpt_correction_T_max  0.3390
_exptl_absorpt_correction_T_min  0.2126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Psi Scan Reflections used    Mu * R = 0.47

H   K   L   2Theta   Chi   Imin/Imax
-4   2   3    17.4    83.7    0.704
4  -2  -3    17.4   -83.7    0.681
5  -2  -4    21.7   -86.3    0.699
-5   2   4    21.7    86.3    0.702
-6   2   3    24.7    82.4    0.721
6  -2  -3    24.7   -82.4    0.727
-6   0   5    25.3    80.4    0.710
6   0  -5    25.3   -80.4    0.724
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         10075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.097
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+8.7714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                7752
_reflns_number_total             10075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b404322g.txt
_cod_data_source_block           JDK27
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014233