σ-Borane Complexes of Iridium: Synthesis and Structural Characterization
Travis J. Hebden; Melanie C. Denney; Vincent Pons; Paula M. B. Piccoli; Thomas F. Koetzle; Arthur J. Schultz; Werner Kaminsky; Karen I. Goldberg; D. Michael Heinekey; Journal of the American Chemical Society 130 (2008) 10812–10820; doi:10.1021/ja801898m

data_4108171
_publ_contact_author_address
;
Intense Pulsed Neutron Source
Argonne National Laboratory
Argonne IL 60439
;
_publ_contact_author_email       ajschultz@anl.gov
_publ_contact_author_fax         1(630)2523465
_publ_contact_author_name        'Schultz, Arthur J.'
_publ_contact_author_phone       1(630)2524163
_publ_section_title
;
 \s-Borane Complexes of Iridium: Synthesis and Structural Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10812
_journal_page_last               10820
_journal_paper_doi               10.1021/ja801898m
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C22 H44 B Ir O2 P2'
_chemical_formula_weight         605.57
_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'
_audit_author_name               'Paula M. B. Piccoli'
_audit_creation_date             2007-10-25T14:56
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2007-10-25T14:56  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                100.215(30)
_cell_angle_beta                 95.23(4)
_cell_angle_gamma                104.52(4)
_cell_formula_units_Z            2
_cell_length_a                   8.262(5)
_cell_length_b                   12.264(5)
_cell_length_c                   13.394(4)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    30(1)
_cell_volume                     1279.8(11)
_computing_cell_refinement       'LATCON (local program)'
_computing_data_collection
;
IPNS SCD time-of-flight neutron Laue diffractometer   (Schultz <i>et al.</i>,
1984)
;
_computing_data_reduction        'ANVRED (local program)'
_computing_structure_refinement  'GSAS (Larson & Von Dreele, 2004)'
_diffrn_ambient_temperature      30(1)
_diffrn_measured_fraction_theta_full 'not applicable to TOF Laue technique'
_diffrn_measured_fraction_theta_max 'not applicable to TOF Laue technique'
_diffrn_measurement_device_type  'IPNS single crystal diffractometer'
_diffrn_measurement_method       'Time-of-flight Laue'
_diffrn_radiation_monochromator  'not applicable to TOF Laue technique'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'Intense Pulsed Neutron Source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.7-4.2
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7349
_diffrn_reflns_theta_full        'not applicable to TOF Laue technique'
_diffrn_reflns_theta_max         'not applicable to TOF Laue technique'
_diffrn_reflns_theta_min         'not applicable to TOF Laue technique'
_exptl_absorpt_coefficient_mu    '1.692 + 2.400\l cm^-1^'
_exptl_absorpt_correction_T_max  0.6213
_exptl_absorpt_correction_T_min  0.0755
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'IPNS ANVRED; (local program)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       irregular
_exptl_crystal_size_max          4
_exptl_crystal_size_mid          3
_exptl_crystal_size_min          0.5
_pd_block_id
2007-10-25T14:56|IRHBH2_phase1|Paula_M._B._Piccoli||
_pd_phase_name                   '(POCOP)Ir(H)2(BH3) at 30 K'
_refine_diff_density_max         '0.771 fm \%A^-3'
_refine_diff_density_min         '-1.997 fm \%A^-3'
_refine_ls_extinction_coef       '6.3(8) x 10^-6'
_refine_ls_extinction_method     Lorentzian-type-I
_refine_ls_goodness_of_fit_all   2.54
_refine_ls_goodness_of_fit_ref   2.54
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         1041
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.197
_refine_ls_R_factor_gt           0.186
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\sFo^2^]^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.189
_reflns_d_resolution_high        0.494
_reflns_d_resolution_low         7.898
_reflns_limit_h_max              8
_reflns_limit_h_min              -16
_reflns_limit_k_max              24
_reflns_limit_k_min              -17
_reflns_limit_l_max              26
_reflns_limit_l_min              -27
_reflns_number_gt                1041
_reflns_number_total             1332
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            ja801898m-file002.cif
_cod_data_source_block           IRHBH2_publ
_cod_original_cell_volume        1256.2(10)
_cod_original_formula_sum        'C22 H44 Ir1 B1 O2 P2'
_cod_database_code               4108171
_cod_database_fobs_code          4108171