#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/45/2004540.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004540
loop_
_publ_author_name
'Grotjahn, D. B.'
'Lo, H. C.'
'Groy, T. L.'
_publ_section_title
Chlorohydrido[2(1H)-pyridonato-N,O]bis[tris(1-methylethyl)phosphine]iridium(III)
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              300
_journal_page_last               302
_journal_paper_doi               10.1107/S0108270195003507
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         '[Ir Cl H (C5 H4 N O) (C9 H21 P)2]'
_chemical_formula_sum            'C23 H47 Cl Ir N O P2'
_chemical_formula_weight         643.2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_type_scat_source           'XLS3 (IntTabIV)'
_cell_angle_alpha                90
_cell_angle_beta                 100.14(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.660(3)
_cell_length_b                   8.940(2)
_cell_length_c                   23.207(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     2789.8(12)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3782
_diffrn_reflns_theta_max         22.5
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 47
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.010
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale amber'
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       parallelepiped
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         '0.98 (<1.5\%A from Ir)'
_refine_diff_density_min         -0.63
_refine_ls_extinction_coef       '\c = 6(2) \\times 10^-5^'
_refine_ls_extinction_method     'F^*^ = F[1 + 0.002\cF²/sin(2θ)]^-1/4^'
_refine_ls_goodness_of_fit_obs   0.83
_refine_ls_hydrogen_treatment
'H atoms refined as riding on their bonding partners'
_refine_ls_number_parameters     263
_refine_ls_number_reflns         2727
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0020F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0472
_reflns_number_observed          2727
_reflns_number_total             3670
_reflns_observed_criterion       F>4.0\s(F)
_cod_data_source_file            sz1010.cif
_cod_data_source_block           sz1010a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(F) + 0.0020F^2^]'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/[\s^2^(F) +
0.0020F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2004540
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,1/2-y,1/2+z
-x,-y,-z
-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Ir .25390(10) .14120(10) .11610(10) .0370(10)
Cl .3420(2) -.0745(3) .09440(10) .0560(10)
P(1) .1465(2) -.0049(3) .16090(10) .0460(10)
P(2) .3275(2) .2859(3) .05120(10) .0400(10)
O .2000(5) .3347(8) .1514(3) .048(3)
N .3401(5) .2300(9) .1987(3) .036(3)
C(1) .4202(8) .2223(14) .2408(4) .053(4)
C(2) .4329(9) .3219(14) .2864(5) .064(5)
C(3) .3649(10) .4322(17) .2877(5) .071(5)
C(4) .2811(9) .4457(13) .2444(5) .059(4)
C(5) .2716(8) .3400(11) .1974(5) .048(4)
C(11) .1943(11) .0507(18) .2840(5) .099(7)
C(12) .1908(9) -.0711(15) .2379(5) .068(5)
C(13) .2923(11) -0.1451(16) .2407(6) .091(6)
C(14) .0716(12) -0.1620(16) .0563(5) .100(7)
C(15) .1155(9) -0.1831(12) .1210(5) .059(4)
C(16) .0551(11) -0.3014(16) .1471(6) .097(7)
C(17) -.0455(9) .0167(18) .1951(6) .094(7)
C(18) .0329(9) .0984(14) .1663(6) .067(5)
C(19) -.0171(9) .1741(19) .1106(6) .095(7)
C(21) .5264(8) .2378(17) .0991(5) .073(5)
C(22) .4530(7) .3636(13) .0777(4) .052(4)
C(23) .4540(9) .4864(13) .1249(5) .066(5)
C(24) .2562(9) .1037(18) -.0483(6) .096(7)
C(25) .3477(8) .1743(13) -.0134(5) .056(4)
C(26) .4090(10) .244(2) -.0536(5) .096(7)
C(27) .1435(8) .4186(16) .0038(6) .087(6)
C(28) .2509(8) .4546(13) .0281(5) .060(4)
C(29) .2930(9) .5684(14) -.0104(6) .073(5)
H(1A) .4693 .1465 .2391 .065
H(2A) .4891 .3146 .3176 .080
H(3A) .3741 .5029 .3194 .085
H(4A) .2318 .5220 .2449 .070
H(11A) .2178 .0102 .3223 .120
H(11B) .2382 .1291 .2762 .120
H(11C) .1286 .0905 .2824 .120
H(12A) .1452 -0.1462 .2464 .080
H(13A) .3167 -0.1798 .2797 .110
H(13B) .2853 -0.2283 .2141 .110
H(13C) .3385 -0.0743 .2295 .110
H(14A) .0581 -0.2580 .0380 .120
H(14B) .0109 -0.1062 .0530 .120
H(14C) .1178 -0.1085 .0373 .120
H(15A) .1785 -0.2308 .1213 .070
H(16A) .0453 -0.3880 .1223 .110
H(16B) .0888 -0.3299 .1854 .110
H(16C) -0.0083 -0.2584 .1500 .110
H(17A) -0.1013 .0814 .1960 .110
H(17B) -0.0671 -0.0707 .1723 .110
H(17C) -0.0172 -0.0127 .2343 .110
H(18A) .0548 .1794 .1925 .080
H(19A) -0.0750 .2270 .1177 .110
H(19B) .0278 .2430 .0972 .110
H(19C) -0.0366 .0988 .0814 .110
H(21A) .5917 .2778 .114 .090
H(21B) .5041 .1866 .1307 .090
H(21C) .5284 .1690 .0676 .090
H(22A) .4749 .4093 .0448 .060
H(23A) .5199 .5247 .1376 .080
H(23B) .4109 .5662 .1084 .080
H(23C) .4296 .4445 .1578 .080
H(24A) .2736 .0470 -0.0801 .110
H(24B) .2257 .0390 -0.0236 .110
H(24C) .2105 .1816 -0.0635 .110
H(25A) .3871 .0909 .0033 .070
H(26A) .4157 .1764 -0.0846 .110
H(26B) .3759 .3337 -0.0697 .110
H(26C) .4737 .2695 -0.0323 .110
H(27A) .1072 .5094 -0.0067 .100
H(27B) .1418 .3577 -0.0305 .100
H(27C) .1137 .3651 .0321 .100
H(28A) .2485 .5078 .0637 .070
H(29A) .2484 .6516 -0.0192 .090
H(29B) .3566 .6037 .0092 .090
H(29C) .3006 .5191 -0.0461 .090
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl Ir P(1) 91.20(10) yes
P(1) Ir P(2) 165.40(10) yes
P(1) Ir O 89.8(2) yes
Cl Ir N 105.2(2) yes
P(2) Ir N 97.8(2) yes
Ir P(1) C(12) 118.5(4) yes
C(12) P(1) C(15) 102.2(5) yes
C(12) P(1) C(18) 103.2(6) yes
Ir P(2) C(22) 118.1(4) yes
C(22) P(2) C(25) 102.0(5) yes
C(22) P(2) C(28) 103.5(5) yes
Ir O C(5) 94.9(6) yes
Ir N C(5) 88.9(5) yes
N C(1) C(2) 120.6(10) yes
C(2) C(3) C(4) 121.7(12) yes
O C(5) N 113.8(9) yes
N C(5) C(4) 119.5(9) yes
P(1) C(12) C(13) 108.3(9) yes
P(1) C(15) C(14) 113.6(8) yes
C(14) C(15) C(16) 109.2(10) yes
P(1) C(18) C(19) 115.4(10) yes
P(2) C(22) C(21) 110.3(8) yes
C(21) C(22) C(23) 111.6(8) yes
P(2) C(25) C(26) 117.1(9) yes
P(2) C(28) C(27) 113.3(9) yes
C(27) C(28) C(29) 111.3(10) yes
Cl Ir P(2) 91.20(10) yes
Cl Ir O 167.6(2) yes
P(2) Ir O 90.9(2) yes
P(1) Ir N 95.4(2) yes
O Ir N 62.4(3) yes
Ir P(1) C(15) 111.4(4) yes
Ir P(1) C(18) 110.8(4) yes
C(15) P(1) C(18) 110.2(5) yes
Ir P(2) C(25) 111.3(4) yes
Ir P(2) C(28) 110.5(4) yes
C(25) P(2) C(28) 110.9(5) yes
Ir N C(1) 149.2(7) yes
C(1) N C(5) 121.9(9) yes
C(1) C(2) C(3) 119.7(10) yes
C(3) C(4) C(5) 116.5(11) yes
O C(5) C(4) 126.6(10) yes
P(1) C(12) C(11) 114.2(9) yes
C(11) C(12) C(13) 111.3(10) yes
P(1) C(15) C(16) 119.2(9) yes
P(1) C(18) C(17) 117.0(9) yes
C(17) C(18) C(19) 109.8(10) yes
P(2) C(22) C(23) 113.1(8) yes
P(2) C(25) C(24) 115.5(9) yes
C(24) C(25) C(26) 110.1(10) yes
P(2) C(28) C(29) 117.3(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ir Cl 2.374(3) yes
Ir P(2) 2.341(3) yes
Ir N 2.214(7) yes
P(1) C(15) 1.854(11) yes
P(2) C(22) 1.852(10) yes
P(2) C(28) 1.860(12) yes
N C(1) 1.334(12) yes
C(1) C(2) 1.370(17) yes
C(3) C(4) 1.390(16) yes
C(11) C(12) 1.522(19) yes
C(14) C(15) 1.527(15) yes
C(17) C(18) 1.54(2) yes
C(21) C(22) 1.529(17) yes
C(24) C(25) 1.503(16) yes
C(27) C(28) 1.511(15) yes
Ir P(1) 2.339(3) yes
Ir O 2.102(7) yes
P(1) C(12) 1.879(12) yes
P(1) C(18) 1.829(13) yes
P(2) C(25) 1.863(12) yes
O C(5) 1.316(12) yes
N C(5) 1.354(13) yes
C(2) C(3) 1.359(19) yes
C(4) C(5) 1.430(16) yes
C(12) C(13) 1.53(2) yes
C(15) C(16) 1.530(19) yes
C(18) C(19) 1.511(18) yes
C(22) C(23) 1.550(16) yes
C(25) C(26) 1.495(19) yes
C(28) C(29) 1.531(18) yes
Ir C(5) 2.573(11) no
C(1) H(1A) 0.960 no
C(2) H(2A) 0.960 no
C(3) H(3A) 0.960 no
C(4) H(4A) 0.960 no
C(11) H(11A) 0.960 no
C(11) H(11B) 0.960 no
C(11) H(11C) 0.960 no
C(12) H(12A) 0.960 no
C(13) H(13A) 0.960 no
C(13) H(13B) 0.960 no
C(13) H(13C) 0.960 no
C(14) H(14A) 0.960 no
C(14) H(14B) 0.960 no
C(14) H(14C) 0.960 no
C(15) H(15A) 0.960 no
C(16) H(16A) 0.960 no
C(16) H(16B) 0.960 no
C(16) H(16C) 0.960 no
C(17) H(17A) 0.960 no
C(17) H(17B) 0.960 no
C(17) H(17C) 0.960 no
C(18) H(18A) 0.960 no
C(19) H(19A) 0.960 no
C(19) H(19B) 0.960 no
C(19) H(19C) 0.960 no
C(21) H(21A) 0.960 no
C(21) H(21B) 0.960 no
C(21) H(21C) 0.960 no
C(22) H(22A) 0.960 no
C(23) H(23A) 0.960 no
C(23) H(23B) 0.960 no
C(23) H(23C) 0.960 no
C(24) H(24A) 0.960 no
C(24) H(24B) 0.960 no
C(24) H(24C) 0.960 no
C(25) H(25A) 0.960 no
C(26) H(26A) 0.960 no
C(26) H(26B) 0.960 no
C(26) H(26C) 0.960 no
C(27) H(27A) 0.960 no
C(27) H(27B) 0.960 no
C(27) H(27C) 0.960 no
C(28) H(28A) 0.960 no
C(29) H(29A) 0.960 no
C(29) H(29B) 0.960 no
C(29) H(29C) 0.960 no
