#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:06:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178768 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/22/4102284.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_4102284
loop_
_publ_author_name
'Fu Chen'
'Guibin Ma'
'Guy M. Bernard'
'Ronald G. Cavell'
'Robert McDonald'
'Michael J. Ferguson'
'Roderick E. Wasylishen'
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton, Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       Roderick.Wasylishen@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr. Roderick E. Wasylishen'
_publ_contact_author_phone       1(780)4924336
_publ_section_title
;
 Solid-State 115In and 31P NMR Studies of Triarylphosphine Indium
 Trihalide Adducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5479
_journal_page_last               5493
_journal_paper_doi               10.1021/ja100625p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C21 H21 I3 In O3 P'
_chemical_formula_sum            'C21 H21 I3 In O3 P'
_chemical_formula_weight         847.87
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.5747(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6759(17)
_cell_length_b                   23.230(3)
_cell_length_c                   8.6375(11)
_cell_measurement_reflns_used    7984
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.41
_cell_volume                     2688.3(6)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       'ω scans'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11546
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.402
_exptl_absorpt_correction_T_max  0.5581
_exptl_absorpt_correction_T_min  0.2315
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0425
_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/[σ²(Fo²)+(0.0588P)²+1.3472P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                5493
_reflns_number_total             6113
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja100625p_si_010.cif
_cod_data_source_block           I3In[P(p-Anis)3](7)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4102284
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.28624(5) 0.16851(4) -0.13073(9) 0.0789(2) Uani 1 1 d .
I2 I -0.02699(4) 0.23376(2) -0.25458(6) 0.05015(14) Uani 1 1 d .
I3 I 0.03088(5) 0.04652(2) -0.13960(7) 0.05999(17) Uani 1 1 d .
In In 0.09750(4) 0.15540(2) -0.09263(5) 0.03853(12) Uani 1 1 d .
P P 0.10476(13) 0.17304(7) 0.2032(2) 0.0330(3) Uani 1 1 d .
O1 O -0.2685(4) 0.1000(2) 0.3989(7) 0.0475(12) Uani 1 1 d .
O2 O 0.4613(5) 0.0457(3) 0.5401(9) 0.0654(18) Uani 1 1 d .
O3 O 0.1520(5) 0.4194(2) 0.3791(9) 0.0591(15) Uani 1 1 d .
C11 C -0.0090(5) 0.1484(3) 0.2567(9) 0.0347(14) Uani 1 1 d .
C12 C -0.0983(6) 0.1669(4) 0.1721(10) 0.0467(18) Uani 1 1 d .
H12 H -0.0997 0.1904 0.0817 0.056 Uiso 1 1 calc R
C13 C -0.1886(6) 0.1518(4) 0.2158(10) 0.0452(17) Uani 1 1 d .
H13 H -0.2508 0.1648 0.1564 0.054 Uiso 1 1 calc R
C14 C -0.1840(6) 0.1177(3) 0.3475(9) 0.0380(15) Uani 1 1 d .
C15 C -0.0961(6) 0.0973(3) 0.4331(9) 0.0431(16) Uani 1 1 d .
H15 H -0.0957 0.0725 0.5208 0.052 Uiso 1 1 calc R
C16 C -0.0076(5) 0.1131(3) 0.3906(8) 0.0379(14) Uani 1 1 d .
H16 H 0.0542 0.1002 0.4515 0.045 Uiso 1 1 calc R
C17 C -0.3608(7) 0.1227(5) 0.3278(11) 0.063(2) Uani 1 1 d .
H17A H -0.3761 0.1120 0.2158 0.076 Uiso 1 1 calc R
H17B H -0.3589 0.1647 0.3373 0.076 Uiso 1 1 calc R
H17C H -0.4126 0.1074 0.3802 0.076 Uiso 1 1 calc R
C21 C 0.2090(5) 0.1350(3) 0.3133(8) 0.0367(14) Uani 1 1 d .
C22 C 0.2160(7) 0.0756(3) 0.2884(12) 0.0511(19) Uani 1 1 d .
H22 H 0.1632 0.0568 0.2186 0.061 Uiso 1 1 calc R
C23 C 0.2983(6) 0.0432(3) 0.3631(11) 0.0488(19) Uani 1 1 d .
H23 H 0.3008 0.0027 0.3473 0.059 Uiso 1 1 calc R
C24 C 0.3756(6) 0.0714(4) 0.4601(10) 0.0451(17) Uani 1 1 d .
C25 C 0.3729(7) 0.1310(4) 0.4859(10) 0.052(2) Uani 1 1 d .
H25 H 0.4263 0.1499 0.5544 0.063 Uiso 1 1 calc R
C26 C 0.2885(6) 0.1622(3) 0.4072(10) 0.0424(16) Uani 1 1 d .
H26 H 0.2868 0.2028 0.4197 0.051 Uiso 1 1 calc R
C27 C 0.4689(10) -0.0154(6) 0.5208(18) 0.091(4) Uani 1 1 d .
H27A H 0.4458 -0.0254 0.4092 0.109 Uiso 1 1 calc R
H27B H 0.4275 -0.0351 0.5846 0.109 Uiso 1 1 calc R
H27C H 0.5386 -0.0273 0.5553 0.109 Uiso 1 1 calc R
C31 C 0.1185(5) 0.2485(3) 0.2527(8) 0.0338(13) Uani 1 1 d .
C32 C 0.1865(6) 0.2805(3) 0.1965(9) 0.0428(17) Uani 1 1 d .
H32 H 0.2238 0.2630 0.1277 0.051 Uiso 1 1 calc R
C33 C 0.2034(7) 0.3377(3) 0.2358(10) 0.0475(19) Uani 1 1 d .
H33 H 0.2537 0.3589 0.1991 0.057 Uiso 1 1 calc R
C34 C 0.1438(6) 0.3639(3) 0.3321(9) 0.0412(15) Uani 1 1 d .
C35 C 0.0726(6) 0.3322(3) 0.3842(10) 0.0463(18) Uani 1 1 d .
H35 H 0.0314 0.3501 0.4466 0.056 Uiso 1 1 calc R
C36 C 0.0599(6) 0.2743(3) 0.3470(10) 0.0434(16) Uani 1 1 d .
H36 H 0.0114 0.2524 0.3859 0.052 Uiso 1 1 calc R
C37 C 0.2255(11) 0.4538(5) 0.331(2) 0.094(5) Uani 1 1 d .
H37A H 0.2335 0.4418 0.2252 0.112 Uiso 1 1 calc R
H37B H 0.2891 0.4492 0.4057 0.112 Uiso 1 1 calc R
H37C H 0.2050 0.4943 0.3278 0.112 Uiso 1 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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
P In I1 104.92(5)
P In I2 107.68(4)
I1 In I2 112.57(3)
P In I3 104.13(4)
I1 In I3 113.14(3)
I2 In I3 113.48(3)
C21 P C11 110.2(3)
C21 P C31 108.7(3)
C11 P C31 107.5(3)
C21 P In 108.6(2)
C11 P In 110.0(2)
C31 P In 111.8(2)
C14 O1 C17 119.3(7)
C24 O2 C27 116.5(9)
C34 O3 C37 118.2(8)
C12 C11 C16 119.0(7)
C12 C11 P 119.3(5)
C16 C11 P 121.5(5)
C11 C12 C13 121.3(7)
C14 C13 C12 117.9(7)
C15 C14 C13 122.5(7)
C15 C14 O1 115.2(7)
C13 C14 O1 122.3(7)
C14 C15 C16 119.1(7)
C15 C16 C11 120.1(7)
C26 C21 C22 118.2(7)
C26 C21 P 122.8(6)
C22 C21 P 118.6(6)
C23 C22 C21 122.2(8)
C24 C23 C22 118.1(7)
O2 C24 C23 124.9(8)
O2 C24 C25 113.3(8)
C23 C24 C25 121.8(7)
C24 C25 C26 118.2(8)
C21 C26 C25 121.4(7)
C32 C31 C36 119.4(7)
C32 C31 P 119.6(5)
C36 C31 P 120.9(5)
C31 C32 C33 122.3(7)
C32 C33 C34 118.1(7)
O3 C34 C35 115.9(7)
O3 C34 C33 124.4(7)
C35 C34 C33 119.7(7)
C34 C35 C36 120.7(7)
C35 C36 C31 119.7(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
I1 In 2.6841(8)
I2 In 2.6859(7)
I3 In 2.6912(8)
In P 2.5698(18)
P C21 1.781(7)
P C11 1.802(7)
P C31 1.806(7)
O1 C14 1.381(9)
O1 C17 1.393(11)
O2 C24 1.373(10)
O2 C27 1.435(15)
O3 C34 1.351(9)
O3 C37 1.411(13)
C11 C12 1.361(11)
C11 C16 1.416(10)
C12 C13 1.406(11)
C13 C14 1.378(11)
C14 C15 1.363(11)
C15 C16 1.383(10)
C21 C26 1.373(11)
C21 C22 1.403(10)
C22 C23 1.400(12)
C23 C24 1.376(12)
C24 C25 1.404(13)
C25 C26 1.416(11)
C31 C32 1.354(10)
C31 C36 1.388(10)
C32 C33 1.378(10)
C33 C34 1.414(11)
C34 C35 1.366(11)
C35 C36 1.386(11)
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
I1 In P C21 -45.1(3)
I2 In P C21 -165.2(3)
I3 In P C21 74.0(3)
I1 In P C11 -165.7(2)
I2 In P C11 74.1(2)
I3 In P C11 -46.6(2)
I1 In P C31 74.9(2)
I2 In P C31 -45.2(2)
I3 In P C31 -166.0(2)
C21 P C11 C12 -171.8(6)
C31 P C11 C12 69.8(7)
In P C11 C12 -52.2(6)
C21 P C11 C16 12.0(7)
C31 P C11 C16 -106.3(6)
In P C11 C16 131.7(5)
C16 C11 C12 C13 0.4(12)
P C11 C12 C13 -175.8(6)
C11 C12 C13 C14 0.0(12)
C12 C13 C14 C15 -1.6(12)
C12 C13 C14 O1 -179.2(7)
C17 O1 C14 C15 174.3(8)
C17 O1 C14 C13 -8.0(11)
C13 C14 C15 C16 2.6(12)
O1 C14 C15 C16 -179.6(7)
C14 C15 C16 C11 -2.1(11)
C12 C11 C16 C15 0.6(11)
P C11 C16 C15 176.8(6)
C11 P C21 C26 -122.9(6)
C31 P C21 C26 -5.3(7)
In P C21 C26 116.6(6)
C11 P C21 C22 65.0(7)
C31 P C21 C22 -177.4(6)
In P C21 C22 -55.5(7)
C26 C21 C22 C23 3.8(12)
P C21 C22 C23 176.2(7)
C21 C22 C23 C24 -2.0(13)
C27 O2 C24 C23 -0.7(14)
C27 O2 C24 C25 179.3(9)
C22 C23 C24 O2 -179.4(8)
C22 C23 C24 C25 0.5(13)
O2 C24 C25 C26 179.0(7)
C23 C24 C25 C26 -0.9(13)
C22 C21 C26 C25 -4.1(12)
P C21 C26 C25 -176.2(6)
C24 C25 C26 C21 2.8(12)
C21 P C31 C32 73.9(7)
C11 P C31 C32 -166.8(6)
In P C31 C32 -46.0(7)
C21 P C31 C36 -106.5(7)
C11 P C31 C36 12.8(7)
In P C31 C36 133.6(6)
C36 C31 C32 C33 3.2(12)
P C31 C32 C33 -177.2(7)
C31 C32 C33 C34 -3.0(13)
C37 O3 C34 C35 179.0(11)
C37 O3 C34 C33 -0.7(15)
C32 C33 C34 O3 -179.8(8)
C32 C33 C34 C35 0.5(12)
O3 C34 C35 C36 -178.0(8)
C33 C34 C35 C36 1.7(12)
C34 C35 C36 C31 -1.5(13)
C32 C31 C36 C35 -0.9(12)
P C31 C36 C35 179.5(6)
