data_2203181
loop_
_publ_author_name
'Jonathan P. H. Charmant'
'Nicholas C. Norman'
'A. Guy Orpen'
'George R. Whittell'
_publ_section_title
;
Carbonyldichlorohydridobis(trimethylphosphine)iridium(III)
;
_journal_issue                 2
_journal_name_full             'Acta Crystallographica, Section E'
_journal_page_first            m164
_journal_page_last             m165
_journal_volume                60
_journal_year                  2004
_chemical_formula_iupac        '[Ir Cl2 H (C3 H9 P)2 (C O)]'
_chemical_formula_moiety       'C7 H19 Cl2 Ir O P2'
_chemical_formula_sum          'C7 H19 Cl2 Ir O P2'
_chemical_formula_weight       444.26
_symmetry_cell_setting         Monoclinic
_symmetry_space_group_name_Hall 'P -2yac'
_symmetry_space_group_name_H-M 'P n'
_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               97.157(5)
_cell_angle_gamma              90.00
_cell_formula_units_Z          2
_cell_length_a                 6.472(2)
_cell_length_b                 13.156(4)
_cell_length_c                 8.598(3)
_cell_measurement_reflns_used  5819
_cell_measurement_temperature  173(2)
_cell_measurement_theta_max    40
_cell_measurement_theta_min    2
_cell_volume                   726.4(4)
_computing_cell_refinement     'SAINT (Bruker, 1996)'
_computing_data_collection     'SMART (Bruker, 1996)'
_computing_data_reduction      'SHELXTL (Bruker, 2001) and SAINT'
_computing_molecular_graphics  SHELXTL
_computing_publication_material SHELXTL
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution  'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature    173(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker SMART CCD area-detector'
_diffrn_measurement_method     'frames, each covering 0.3\% in \w'
_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 0.0747
_diffrn_reflns_av_sigmaI/netI  0.0898
_diffrn_reflns_limit_h_max     8
_diffrn_reflns_limit_h_min     -8
_diffrn_reflns_limit_k_max     17
_diffrn_reflns_limit_k_min     -16
_diffrn_reflns_limit_l_max     11
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_number          7494
_diffrn_reflns_theta_full      27.57
_diffrn_reflns_theta_max       27.57
_diffrn_reflns_theta_min       1.55
_diffrn_standards_decay_%      0
_exptl_absorpt_coefficient_mu  9.747
_exptl_absorpt_correction_T_max 0.613
_exptl_absorpt_correction_T_min 0.310
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour          orange
_exptl_crystal_density_diffrn  2.031
_exptl_crystal_density_method  'not measured'
_exptl_crystal_description     block
_exptl_crystal_F_000           420
_exptl_crystal_size_max        0.20
_exptl_crystal_size_mid        0.10
_exptl_crystal_size_min        0.05
_refine_diff_density_max       2.697
_refine_diff_density_min       -3.569
_refine_ls_abs_structure_details 'Flack (1983), 1482 Friedel pairs'
_refine_ls_abs_structure_Flack 0.149(13)
_refine_ls_extinction_method   none
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_hydrogen_treatment  mixed
_refine_ls_matrix_type         full
_refine_ls_number_parameters   128
_refine_ls_number_reflns       3176
_refine_ls_number_restraints   3
_refine_ls_restrained_S_all    1.054
_refine_ls_R_factor_all        0.0454
_refine_ls_R_factor_gt         0.0424
_refine_ls_shift/su_max        0.000
_refine_ls_shift/su_mean       0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0144P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme    calc
_refine_ls_wR_factor_gt        0.0975
_refine_ls_wR_factor_ref       0.0997
_reflns_number_gt              2964
_reflns_number_total           3176
_reflns_threshold_expression   I>2\s(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y, z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1 1.0420(13) 0.3113(7) 0.7435(10) 0.0320(17) Uani d . 1 . . C
C2 1.1657(18) 0.4692(7) 1.0321(11) 0.049(2) Uani d . 1 . . C
H2A 1.2090 0.5129 1.1227 0.073 Uiso calc R 1 . . H
H2B 1.0541 0.5027 0.9632 0.073 Uiso calc R 1 . . H
H2C 1.2847 0.4570 0.9744 0.073 Uiso calc R 1 . . H
C3 1.2949(16) 0.2941(8) 1.2214(12) 0.046(2) Uani d . 1 . . C
H3A 1.4056 0.2788 1.1569 0.070 Uiso calc R 1 . . H
H3B 1.2511 0.2313 1.2690 0.070 Uiso calc R 1 . . H
H3C 1.3471 0.3423 1.3040 0.070 Uiso calc R 1 . . H
C4 0.8931(15) 0.3871(7) 1.2353(12) 0.041(2) Uani d . 1 . . C
H4A 0.9711 0.4178 1.3286 0.062 Uiso calc R 1 . . H
H4B 0.8185 0.3269 1.2659 0.062 Uiso calc R 1 . . H
H4C 0.7929 0.4365 1.1850 0.062 Uiso calc R 1 . . H
C5 0.786(3) 0.1484(13) 0.5178(13) 0.106(7) Uani d . 1 . . C
H5A 0.9322 0.1379 0.5025 0.159 Uiso calc R 1 . . H
H5B 0.7452 0.2183 0.4891 0.159 Uiso calc R 1 . . H
H5C 0.6980 0.1008 0.4515 0.159 Uiso calc R 1 . . H
C6 0.831(3) -0.0049(9) 0.7503(18) 0.085(4) Uani d . 1 . . C
H6A 0.7468 -0.0486 0.6748 0.127 Uiso calc R 1 . . H
H6B 0.8083 -0.0240 0.8570 0.127 Uiso calc R 1 . . H
H6C 0.9787 -0.0132 0.7381 0.127 Uiso calc R 1 . . H
C7 0.4731(17) 0.1223(10) 0.7128(17) 0.074(4) Uani d . 1 . . C
H7A 0.4100 0.1827 0.6597 0.112 Uiso calc R 1 . . H
H7B 0.4393 0.1204 0.8208 0.112 Uiso calc R 1 . . H
H7C 0.4184 0.0612 0.6570 0.112 Uiso calc R 1 . . H
Cl1 0.6100(4) 0.35400(16) 0.8662(3) 0.0414(5) Uani d . 1 . . Cl
Cl2 0.7829(4) 0.14469(16) 1.0945(3) 0.0403(5) Uani d . 1 . . Cl
Ir1 0.92263(18) 0.242795(17) 0.89647(15) 0.02626(11) Uani d D 1 . . Ir
O1 1.1115(11) 0.3544(6) 0.6500(8) 0.0538(18) Uani d . 1 . . O
P1 1.0728(3) 0.35008(16) 1.0984(3) 0.0307(4) Uani d . 1 . . P
P2 0.7558(4) 0.12727(18) 0.7147(3) 0.0365(5) Uani d . 1 . . P
H1 1.135(10) 0.179(7) 0.917(11) 0.055 Uiso d D 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.030(4) 0.035(5) 0.032(4) 0.003(3) 0.007(3) 0.000(3)
C2 0.068(6) 0.020(4) 0.064(6) -0.009(4) 0.030(5) -0.005(4)
C3 0.042(5) 0.044(6) 0.051(5) 0.000(4) -0.001(4) -0.005(5)
C4 0.043(5) 0.028(4) 0.058(5) -0.002(4) 0.023(4) -0.011(4)
C5 0.159(17) 0.104(13) 0.049(8) -0.069(12) -0.009(9) 0.001(7)
C6 0.102(10) 0.037(6) 0.105(10) 0.028(7) -0.026(8) -0.032(7)
C7 0.046(6) 0.058(8) 0.116(11) -0.010(5) 0.000(7) -0.040(7)
Cl1 0.0392(11) 0.0245(10) 0.0613(13) 0.0097(8) 0.0102(10) 0.0045(9)
Cl2 0.0568(13) 0.0218(10) 0.0443(11) -0.0015(9) 0.0147(10) 0.0042(8)
Ir1 0.02997(17) 0.01981(15) 0.03020(16) 0.0048(2) 0.00845(12) 0.0010(3)
O1 0.053(4) 0.054(5) 0.055(4) -0.003(3) 0.009(3) 0.015(3)
P1 0.0358(11) 0.0192(10) 0.0389(11) -0.0025(8) 0.0119(9) -0.0018(8)
P2 0.0427(12) 0.0279(12) 0.0385(11) 0.0043(9) 0.0035(10) -0.0019(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 Ir1 . . 178.6(8) no
P1 C2 H2A . . 109.5 no
P1 C2 H2B . . 109.5 no
H2A C2 H2B . . 109.5 no
P1 C2 H2C . . 109.5 no
H2A C2 H2C . . 109.5 no
H2B C2 H2C . . 109.5 no
P1 C3 H3A . . 109.5 no
P1 C3 H3B . . 109.5 no
H3A C3 H3B . . 109.5 no
P1 C3 H3C . . 109.5 no
H3A C3 H3C . . 109.5 no
H3B C3 H3C . . 109.5 no
P1 C4 H4A . . 109.5 no
P1 C4 H4B . . 109.5 no
H4A C4 H4B . . 109.5 no
P1 C4 H4C . . 109.5 no
H4A C4 H4C . . 109.5 no
H4B C4 H4C . . 109.5 no
P2 C5 H5A . . 109.5 no
P2 C5 H5B . . 109.5 no
H5A C5 H5B . . 109.5 no
P2 C5 H5C . . 109.5 no
H5A C5 H5C . . 109.5 no
H5B C5 H5C . . 109.5 no
P2 C6 H6A . . 109.5 no
P2 C6 H6B . . 109.5 no
H6A C6 H6B . . 109.5 no
P2 C6 H6C . . 109.5 no
H6A C6 H6C . . 109.5 no
H6B C6 H6C . . 109.5 no
P2 C7 H7A . . 109.5 no
P2 C7 H7B . . 109.5 no
H7A C7 H7B . . 109.5 no
P2 C7 H7C . . 109.5 no
H7A C7 H7C . . 109.5 no
H7B C7 H7C . . 109.5 no
C1 Ir1 P2 . . 92.3(3) yes
C1 Ir1 P1 . . 93.6(3) yes
P2 Ir1 P1 . . 174.11(12) yes
C1 Ir1 Cl2 . . 176.3(3) yes
P2 Ir1 Cl2 . . 86.63(9) yes
P1 Ir1 Cl2 . . 87.51(10) yes
C1 Ir1 Cl1 . . 92.6(3) yes
P2 Ir1 Cl1 . . 90.60(10) yes
P1 Ir1 Cl1 . . 88.86(9) yes
Cl2 Ir1 Cl1 . . 90.98(10) yes
C1 Ir1 H1 . . 84(4) yes
P2 Ir1 H1 . . 93(4) yes
P1 Ir1 H1 . . 88(4) yes
Cl2 Ir1 H1 . . 92(4) yes
Cl1 Ir1 H1 . . 176(4) yes
C2 P1 C4 . . 103.7(4) no
C2 P1 C3 . . 105.3(5) no
C4 P1 C3 . . 104.7(5) no
C2 P1 Ir1 . . 114.4(3) no
C4 P1 Ir1 . . 113.5(3) no
C3 P1 Ir1 . . 114.1(3) no
C5 P2 C6 . . 104.7(9) no
C5 P2 C7 . . 103.3(8) no
C6 P2 C7 . . 102.4(7) no
C5 P2 Ir1 . . 116.3(5) no
C6 P2 Ir1 . . 114.6(4) no
C7 P2 Ir1 . . 114.0(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 . 1.123(11) no
C1 Ir1 . 1.842(9) yes
C2 P1 . 1.797(9) no
C2 H2A . 0.9800 no
C2 H2B . 0.9800 no
C2 H2C . 0.9800 no
C3 P1 . 1.830(10) yes
C3 H3A . 0.9800 no
C3 H3B . 0.9800 no
C3 H3C . 0.9800 no
C4 P1 . 1.821(9) yes
C4 H4A . 0.9800 no
C4 H4B . 0.9800 no
C4 H4C . 0.9800 no
C5 P2 . 1.751(12) yes
C5 H5A . 0.9800 no
C5 H5B . 0.9800 no
C5 H5C . 0.9800 no
C6 P2 . 1.821(12) yes
C6 H6A . 0.9800 no
C6 H6B . 0.9800 no
C6 H6C . 0.9800 no
C7 P2 . 1.829(12) yes
C7 H7A . 0.9800 no
C7 H7B . 0.9800 no
C7 H7C . 0.9800 no
Cl1 Ir1 . 2.484(2) yes
Cl2 Ir1 . 2.401(3) yes
Ir1 P2 . 2.345(3) yes
Ir1 P1 . 2.352(3) yes
Ir1 H1 . 1.60(2) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 Ir1 P1 C2 . . . . 17.7(5) no
Cl2 Ir1 P1 C2 . . . . -165.9(4) no
Cl1 Ir1 P1 C2 . . . . -74.8(4) no
C1 Ir1 P1 C4 . . . . 136.5(5) no
Cl2 Ir1 P1 C4 . . . . -47.0(4) no
Cl1 Ir1 P1 C4 . . . . 44.0(4) no
C1 Ir1 P1 C3 . . . . -103.6(5) no
Cl2 Ir1 P1 C3 . . . . 72.8(4) no
Cl1 Ir1 P1 C3 . . . . 163.8(4) no
C1 Ir1 P2 C5 . . . . -3.4(8) no
Cl2 Ir1 P2 C5 . . . . -179.8(8) no
Cl1 Ir1 P2 C5 . . . . 89.3(8) no
C1 Ir1 P2 C6 . . . . 119.2(7) no
Cl2 Ir1 P2 C6 . . . . -57.3(7) no
Cl1 Ir1 P2 C6 . . . . -148.2(7) no
C1 Ir1 P2 C7 . . . . -123.4(6) no
Cl2 Ir1 P2 C7 . . . . 60.2(6) no
Cl1 Ir1 P2 C7 . . . . -30.8(6) no