Experimental Characterization of the Hydride (1)H Shielding Tensors for HIrX2(PR3)2 and HRhCl2(PR3)2: Extremely Shielded Hydride Protons with Unusually Large Magnetic Shielding Anisotropies.
Garbacz, Piotr; Terskikh, Victor V.; Ferguson, Michael J.; Bernard, Guy M.; Kędziorek, Mariusz; Wasylishen, Roderick E.; The journal of physical chemistry. A 118 (2014) 1203–1212; doi:10.1021/jp411378j

data_1513341
_publ_section_title
;
 Experimental Characterization of the Hydride (1)H Shielding Tensors for
 HIrX2(PR3)2 and HRhCl2(PR3)2: Extremely Shielded Hydride Protons with
 Unusually Large Magnetic Shielding Anisotropies.
;
_journal_issue                   7
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              1203
_journal_page_last               1212
_journal_paper_doi               10.1021/jp411378j
_journal_volume                  118
_journal_year                    2014
_chemical_formula_moiety         'C18 H43 Cl2 Ir P2'
_chemical_formula_sum            'C18 H43 Cl2 Ir P2'
_chemical_formula_weight         584.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.6720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0646(4)
_cell_length_b                   8.9616(4)
_cell_length_c                   16.2738(8)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.51
_cell_volume                     1174.86(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10572
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.291
_diffrn_reflns_theta_min         2.506
_exptl_absorpt_coefficient_mu    6.045
_exptl_absorpt_correction_T_max  0.3581
_exptl_absorpt_correction_T_min  0.1963
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.271
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2884
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0135
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+0.6952P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2668
_reflns_number_total             2884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp411378j_si_001.cif
_cod_data_source_block           rew1303
_cod_database_code               1513341
_shelx_estimated_absorpt_t_min   0.185
_shelx_estimated_absorpt_t_max   0.291
_shelxl_version_number           2013-2
_shelx_res_checksum              81099
_shelx_hkl_checksum              73010