#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:32:37 +0100 (vie 25 de mar de 2016) $
#$Revision: 179795 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/91/7009148.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009148
loop_
_publ_author_name
'Cobley, Christopher J.'
'Ellis, Dianne D.'
'Orpen, A. Guy'
'Pringle, Paul G.'
_publ_section_title
;
 Calix[4]arene derived phosphites: their hydrolytic stability and
 complexes with gold(I), platinum(II,0), palladium(II) and iridium(I)
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1101
_journal_paper_doi               10.1039/a908960h
_journal_year                    2000
_chemical_formula_sum            'C39 H36 Cl Ir O4 P'
_chemical_formula_weight         827.30
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                82.27(2)
_cell_angle_beta                 84.47(2)
_cell_angle_gamma                71.912(14)
_cell_formula_units_Z            2
_cell_length_a                   8.914(2)
_cell_length_b                   10.115(2)
_cell_length_c                   18.556(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1573.3(6)
_computing_cell_refinement       'SMART (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SMART (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10208
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.422
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_F_000             822
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.152
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_obs          0.0288
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0245P)²+5.5201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0724
_refine_ls_wR_factor_obs         0.0672
_reflns_number_observed          6531
_reflns_number_total             6990
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908960h.txt
_cod_data_source_block           13a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+5.5201P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0245P)^2^+5.5201P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1573.3(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009148
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ir1 Ir -0.22163(2) 0.26600(2) 0.359075(8) 0.01919(5) Uani 1 d . .
Cl1 Cl -0.38349(12) 0.40856(11) 0.26748(6) 0.0288(2) Uani 1 d . .
P1 P -0.04349(11) 0.13814(10) 0.28010(5) 0.0161(2) Uani 1 d . .
O1 O 0.3444(4) 0.2667(4) 0.1954(2) 0.0420(9) Uani 1 d . .
H1 H 0.4337(4) 0.2582(63) 0.2098(22) 0.063 Uiso 1 calc R .
O2 O 0.0001(3) 0.1949(3) 0.19808(14) 0.0187(5) Uani 1 d . .
O3 O -0.0876(3) 0.0008(3) 0.26811(14) 0.0192(5) Uani 1 d . .
O4 O 0.1247(3) 0.0778(3) 0.31478(14) 0.0182(5) Uani 1 d . .
C1 C 0.2291(5) 0.3422(4) 0.2410(2) 0.0243(8) Uani 1 d . .
C2 C 0.2369(5) 0.3158(4) 0.3166(2) 0.0241(8) Uani 1 d . .
C3 C 0.1232(6) 0.4058(5) 0.3587(3) 0.0315(10) Uani 1 d . .
H3 H 0.1298(6) 0.3938(5) 0.4101(3) 0.038 Uiso 1 calc R .
C4 C 0.0010(6) 0.5122(5) 0.3275(3) 0.0362(11) Uani 1 d . .
H4 H -0.0723(6) 0.5757(5) 0.3570(3) 0.043 Uiso 1 calc R .
C5 C -0.0141(6) 0.5257(5) 0.2530(3) 0.0311(9) Uani 1 d . .
H5 H -0.1020(6) 0.5948(5) 0.2319(3) 0.037 Uiso 1 calc R .
C6 C 0.0983(5) 0.4391(4) 0.2092(2) 0.0232(8) Uani 1 d . .
C7 C 0.0759(5) 0.4403(4) 0.1298(2) 0.0262(9) Uani 1 d . .
H7A H 0.1695(5) 0.3720(4) 0.1085(2) 0.031 Uiso 1 calc R .
H7B H 0.0706(5) 0.5341(4) 0.1045(2) 0.031 Uiso 1 calc R .
C8 C -0.1045(5) 0.2826(4) 0.1457(2) 0.0218(8) Uani 1 d . .
C9 C -0.0704(5) 0.4053(4) 0.1155(2) 0.0236(8) Uani 1 d . .
C10 C -0.1764(6) 0.4970(5) 0.0668(3) 0.0338(10) Uani 1 d . .
H10 H -0.1583(6) 0.5826(5) 0.0468(3) 0.041 Uiso 1 calc R .
C11 C -0.3063(6) 0.4664(5) 0.0472(3) 0.0409(12) Uani 1 d . .
H11 H -0.3789(6) 0.5318(5) 0.0157(3) 0.049 Uiso 1 calc R .
C12 C -0.3294(6) 0.3413(5) 0.0735(3) 0.0354(10) Uani 1 d . .
H12 H -0.4165(6) 0.3190(5) 0.0583(3) 0.042 Uiso 1 calc R .
C13 C -0.2283(5) 0.2447(5) 0.1225(2) 0.0260(8) Uani 1 d . .
C14 C -0.2617(6) 0.1069(5) 0.1461(3) 0.0312(10) Uani 1 d . .
H14A H -0.3105(6) 0.1083(5) 0.1964(3) 0.037 Uiso 1 calc R .
H14B H -0.3391(6) 0.0970(5) 0.1139(3) 0.037 Uiso 1 calc R .
C15 C -0.0282(5) -0.0663(4) 0.2049(2) 0.0217(8) Uani 1 d . .
C16 C -0.1171(6) -0.0174(5) 0.1439(2) 0.0272(9) Uani 1 d . .
C17 C -0.0604(7) -0.0852(5) 0.0817(3) 0.0372(11) Uani 1 d . .
H17 H -0.1184(7) -0.0569(5) 0.0390(3) 0.045 Uiso 1 calc R .
C18 C 0.0797(7) -0.1933(5) 0.0818(3) 0.0394(12) Uani 1 d . .
H18 H 0.1177(7) -0.2371(5) 0.0386(3) 0.047 Uiso 1 calc R .
C19 C 0.1668(6) -0.2396(5) 0.1438(3) 0.0333(10) Uani 1 d . .
H19 H 0.2624(6) -0.3147(5) 0.1429(3) 0.040 Uiso 1 calc R .
C20 C 0.1119(5) -0.1740(4) 0.2076(2) 0.0256(9) Uani 1 d . .
C21 C 0.2006(5) -0.2169(4) 0.2767(2) 0.0267(9) Uani 1 d . .
H21A H 0.2562(5) -0.3186(4) 0.2798(2) 0.032 Uiso 1 calc R .
H21B H 0.1229(5) -0.2005(4) 0.3189(2) 0.032 Uiso 1 calc R .
C22 C 0.2817(5) -0.0035(4) 0.3019(2) 0.0196(7) Uani 1 d . .
C23 C 0.3203(5) -0.1408(4) 0.2828(2) 0.0246(8) Uani 1 d . .
C24 C 0.4815(6) -0.2139(5) 0.2743(3) 0.0341(10) Uani 1 d . .
H24 H 0.5116(6) -0.3053(5) 0.2594(3) 0.041 Uiso 1 calc R .
C25 C 0.5976(6) -0.1578(6) 0.2868(3) 0.0402(12) Uani 1 d . .
H25 H 0.7060(6) -0.2086(6) 0.2792(3) 0.048 Uiso 1 calc R .
C26 C 0.5550(5) -0.0273(5) 0.3105(3) 0.0311(10) Uani 1 d . .
H26 H 0.6353(5) 0.0091(5) 0.3215(3) 0.037 Uiso 1 calc R .
C27 C 0.3965(5) 0.0534(4) 0.3189(2) 0.0225(8) Uani 1 d . .
C28 C 0.3607(5) 0.1913(5) 0.3504(2) 0.0271(9) Uani 1 d . .
H28A H 0.3284(5) 0.1761(5) 0.4026(2) 0.032 Uiso 1 calc R .
H28B H 0.4604(5) 0.2159(5) 0.3478(2) 0.032 Uiso 1 calc R .
C101 C -0.1053(6) 0.2693(6) 0.5113(3) 0.0396(12) Uani 1 d . .
H10A H -0.1554(6) 0.2247(6) 0.5535(3) 0.048 Uiso 1 calc R .
H10B H -0.0031(6) 0.2734(6) 0.5260(3) 0.048 Uiso 1 calc R .
C102 C -0.2115(6) 0.4178(6) 0.4917(3) 0.0405(12) Uani 1 d . .
H10C H -0.2719(6) 0.4537(6) 0.5363(3) 0.049 Uiso 1 calc R .
H10D H -0.1446(6) 0.4784(6) 0.4733(3) 0.049 Uiso 1 calc R .
C103 C -0.3264(5) 0.4274(5) 0.4348(3) 0.0319(10) Uani 1 d . .
H103 H -0.3730(5) 0.5239(5) 0.4102(3) 0.038 Uiso 1 calc R .
C104 C -0.4232(5) 0.3425(5) 0.4392(2) 0.0282(9) Uani 1 d . .
H104 H -0.5271(5) 0.3885(5) 0.4169(2) 0.034 Uiso 1 calc R .
C105 C -0.4274(6) 0.2310(6) 0.5023(3) 0.0380(11) Uani 1 d . .
H10E H -0.5363(6) 0.2246(6) 0.5110(3) 0.046 Uiso 1 calc R .
H10F H -0.3980(6) 0.2585(6) 0.5469(3) 0.046 Uiso 1 calc R .
C106 C -0.3147(6) 0.0879(5) 0.4873(3) 0.0354(10) Uani 1 d . .
H10G H -0.2811(6) 0.0329(5) 0.5345(3) 0.042 Uiso 1 calc R .
H10H H -0.3728(6) 0.0379(5) 0.4638(3) 0.042 Uiso 1 calc R .
C107 C -0.1683(6) 0.0928(5) 0.4394(2) 0.0290(9) Uani 1 d . .
H107 H -0.1082(6) 0.0021(5) 0.4203(2) 0.035 Uiso 1 calc R .
C108 C -0.0738(5) 0.1787(5) 0.4484(2) 0.0299(9) Uani 1 d . .
H108 H 0.0407(5) 0.1384(5) 0.4337(2) 0.036 Uiso 1 calc R .
C203 C -0.4758(8) -0.1195(6) 0.0484(4) 0.053(2) Uani 1 d . .
H203 H -0.4594(8) -0.2021(6) 0.0816(4) 0.064 Uiso 1 calc R .
C201 C -0.6111(7) 0.1222(6) 0.0171(3) 0.0483(13) Uani 1 d . .
H201 H -0.6882(7) 0.2064(6) 0.0288(3) 0.058 Uiso 1 calc R .
C202 C -0.5864(8) 0.0025(7) 0.0660(3) 0.0513(14) Uani 1 d . .
H202 H -0.6454(8) 0.0045(7) 0.1115(3) 0.062 Uiso 1 calc R .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C107 Ir1 C108 39.1(2) . . ?
C107 Ir1 C103 96.5(2) . . ?
C108 Ir1 C103 80.2(2) . . ?
C107 Ir1 C104 81.2(2) . . ?
C108 Ir1 C104 88.5(2) . . ?
C103 Ir1 C104 36.3(2) . . ?
C107 Ir1 P1 89.66(13) . . ?
C108 Ir1 P1 92.44(12) . . ?
C103 Ir1 P1 158.98(13) . . ?
C104 Ir1 P1 164.30(12) . . ?
C107 Ir1 Cl1 150.92(13) . . ?
C108 Ir1 Cl1 167.70(13) . . ?
C103 Ir1 Cl1 89.79(13) . . ?
C104 Ir1 Cl1 87.51(12) . . ?
P1 Ir1 Cl1 94.51(4) . . ?
O4 P1 O3 103.89(15) . . ?
O4 P1 O2 102.95(14) . . ?
O3 P1 O2 101.93(14) . . ?
O4 P1 Ir1 109.72(11) . . ?
O3 P1 Ir1 111.07(11) . . ?
O2 P1 Ir1 125.12(11) . . ?
C8 O2 P1 128.0(3) . . ?
C15 O3 P1 119.8(2) . . ?
C22 O4 P1 143.5(3) . . ?
O1 C1 C6 117.2(4) . . ?
O1 C1 C2 121.3(4) . . ?
C6 C1 C2 121.3(4) . . ?
C3 C2 C1 117.6(4) . . ?
C3 C2 C28 121.8(4) . . ?
C1 C2 C28 120.6(4) . . ?
C4 C3 C2 121.5(4) . . ?
C3 C4 C5 119.5(4) . . ?
C4 C5 C6 120.5(4) . . ?
C5 C6 C1 118.7(4) . . ?
C5 C6 C7 121.6(4) . . ?
C1 C6 C7 119.5(4) . . ?
C6 C7 C9 114.0(4) . . ?
C13 C8 C9 121.7(4) . . ?
C13 C8 O2 122.1(3) . . ?
C9 C8 O2 116.1(3) . . ?
C8 C9 C10 117.2(4) . . ?
C8 C9 C7 123.9(4) . . ?
C10 C9 C7 118.8(4) . . ?
C11 C10 C9 121.8(4) . . ?
C12 C11 C10 119.3(4) . . ?
C11 C12 C13 121.9(4) . . ?
C8 C13 C12 117.6(4) . . ?
C8 C13 C14 125.0(4) . . ?
C12 C13 C14 117.4(4) . . ?
C16 C14 C13 113.3(4) . . ?
C20 C15 C16 124.9(4) . . ?
C20 C15 O3 118.5(4) . . ?
C16 C15 O3 116.6(4) . . ?
C15 C16 C17 116.8(4) . . ?
C15 C16 C14 120.0(4) . . ?
C17 C16 C14 123.1(4) . . ?
C18 C17 C16 120.3(5) . . ?
C17 C18 C19 121.6(4) . . ?
C18 C19 C20 119.4(5) . . ?
C15 C20 C19 117.0(4) . . ?
C15 C20 C21 120.4(4) . . ?
C19 C20 C21 122.6(4) . . ?
C20 C21 C23 114.9(3) . . ?
C27 C22 O4 115.3(3) . . ?
C27 C22 C23 122.2(4) . . ?
O4 C22 C23 122.0(3) . . ?
C24 C23 C22 116.8(4) . . ?
C24 C23 C21 118.6(4) . . ?
C22 C23 C21 124.5(4) . . ?
C25 C24 C23 122.2(4) . . ?
C26 C25 C24 119.3(4) . . ?
C25 C26 C27 121.9(4) . . ?
C22 C27 C26 117.3(4) . . ?
C22 C27 C28 124.5(4) . . ?
C26 C27 C28 118.1(4) . . ?
C2 C28 C27 118.3(3) . . ?
C102 C101 C108 113.0(4) . . ?
C103 C102 C101 113.2(4) . . ?
C104 C103 C102 123.8(5) . . ?
C104 C103 Ir1 72.2(2) . . ?
C102 C103 Ir1 110.4(3) . . ?
C103 C104 C105 123.6(4) . . ?
C103 C104 Ir1 71.5(2) . . ?
C105 C104 Ir1 111.5(3) . . ?
C104 C105 C106 111.9(4) . . ?
C107 C106 C105 114.6(4) . . ?
C108 C107 C106 124.1(4) . . ?
C108 C107 Ir1 71.7(2) . . ?
C106 C107 Ir1 110.7(3) . . ?
C107 C108 C101 122.5(4) . . ?
C107 C108 Ir1 69.3(2) . . ?
C101 C108 Ir1 114.9(3) . . ?
C202 C203 C201 120.2(6) . 2_455 ?
C203 C201 C202 120.1(6) 2_455 . ?
C203 C202 C201 119.7(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C107 2.106(4) . ?
Ir1 C108 2.137(4) . ?
Ir1 C103 2.220(4) . ?
Ir1 C104 2.230(4) . ?
Ir1 P1 2.2644(11) . ?
Ir1 Cl1 2.3605(11) . ?
P1 O4 1.596(3) . ?
P1 O3 1.604(3) . ?
P1 O2 1.608(3) . ?
O1 C1 1.370(5) . ?
O2 C8 1.425(5) . ?
O3 C15 1.410(5) . ?
O4 C22 1.402(5) . ?
C1 C6 1.391(6) . ?
C1 C2 1.395(6) . ?
C2 C3 1.390(6) . ?
C2 C28 1.502(6) . ?
C3 C4 1.380(7) . ?
C4 C5 1.386(7) . ?
C5 C6 1.386(6) . ?
C6 C7 1.505(6) . ?
C7 C9 1.508(6) . ?
C8 C13 1.396(6) . ?
C8 C9 1.401(6) . ?
C9 C10 1.401(6) . ?
C10 C11 1.380(7) . ?
C11 C12 1.363(7) . ?
C12 C13 1.402(6) . ?
C13 C14 1.514(6) . ?
C14 C16 1.497(7) . ?
C15 C20 1.379(6) . ?
C15 C16 1.390(6) . ?
C16 C17 1.395(7) . ?
C17 C18 1.381(8) . ?
C18 C19 1.395(7) . ?
C19 C20 1.407(6) . ?
C20 C21 1.514(6) . ?
C21 C23 1.517(6) . ?
C22 C27 1.399(6) . ?
C22 C23 1.408(6) . ?
C23 C24 1.402(6) . ?
C24 C25 1.377(8) . ?
C25 C26 1.375(7) . ?
C26 C27 1.401(6) . ?
C27 C28 1.515(6) . ?
C101 C102 1.523(8) . ?
C101 C108 1.531(6) . ?
C102 C103 1.513(7) . ?
C103 C104 1.385(7) . ?
C104 C105 1.518(7) . ?
C105 C106 1.527(7) . ?
C106 C107 1.517(6) . ?
C107 C108 1.419(7) . ?
C203 C202 1.375(9) . ?
C203 C201 1.376(9) 2_455 ?
C201 C203 1.376(9) 2_455 ?
C201 C202 1.384(9) . ?
