Unprecedented pentadenticity of the HB(3-Phpz)3 (= TpPh) ligand
Slugovc, Christian; Carmona, Ernesto; Mereiter, Kurt; Trofimenko, Swiatoslaw; Chemical Communications  (2000) 121–; doi:10.1039/a908478i

data_7110772
_publ_section_title
;
 Unprecedented pentadenticity of the HB(3-Phpz)3 (= TpPh) ligand
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              121
_journal_paper_doi               10.1039/a908478i
_journal_year                    2000
_chemical_formula_sum            'C31 H30 B Ir N6'
_chemical_formula_weight         689.62
_chemical_name_common
Ir(\k^4^(N,N,N,C^Ph2^)-Tp^Ph^)(ethyl)(\h^2^-ethene)
_chemical_name_systematic
;
 (\k^4^(N,N',N'',C^Ph2^)-hydrogen tris(3-phenylpyrazol-1-yl)borato)-
 (\k^1^-ethyl)-(\h^2^-ethene)-iridium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.399(5)
_cell_length_b                   8.691(3)
_cell_length_c                   19.809(5)
_cell_measurement_reflns_used    7995
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     2821.9(15)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT and SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
'Siemens SMART 3-circle with CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32315
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    4.763
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 absorption correction by multi-scan method using program SADABS
 (G.M. Sheldrick, 1996)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.702
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00040(5)
_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   1.381
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.381
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+4.5304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                5616
_reflns_number_total             6013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a908478isup1.cif
_cod_data_source_block           cssaj3fr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               7110772