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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/61/4306165.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_4306165
loop_
_publ_author_name
'Fei Cheng'
'Sarah I. Friend'
'Andrew L. Hector'
'William Levason'
'Gillian Reid'
'Michael Webster'
'Wenjian Zhang'
_publ_contact_author_address
;   School of Chemistry
    University of Southampton
    Southampton SO17 1BJ, UK
;
_publ_contact_author_email       wxl@soton.ac.uk
_publ_contact_author_fax         '023 8059 3781'
_publ_contact_author_name        'Professor W. Levason'
_publ_contact_author_phone       '023 8059 3792'
_publ_section_title
;
Preparation, Characterization, and Structural Systematics of Diphosphane
and Diarsane Complexes of Indium(III) Halides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9691
_journal_page_last               9700
_journal_paper_doi               10.1021/ic801091n
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H32 Cl6 In2 P4, 0.6(C H2 Cl2)'
_chemical_formula_sum            'C20.6 H33.2 Cl7.2 In2 P4'
_chemical_formula_weight         889.63
_chemical_name_systematic
; 
 bis((mu₂-chloro)-(1,2-bis(dimethylphosphanyl)benzene)-dichloro-indium(III))
 dichloromethane solvate 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Webster, M.'
_audit_creation_date             2008-01-18
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6164(15)
_cell_length_b                   14.3423(15)
_cell_length_c                   15.836(2)
_cell_measurement_reflns_used    32187
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3546.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26394
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.22
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1749
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.319
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0541
_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/[σ²(Fo²)+(0.0566P)²+22.7460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1433
_reflns_number_gt                3116
_reflns_number_total             4062
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic801091n_si_001_5.cif
_cod_data_source_block           07fc038
_cod_original_formula_sum        'C20.60 H33.20 Cl7.20 In2 P4'
_cod_database_code               4306165
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.54387(2) 0.46426(3) 0.38848(3) 0.02018(14) Uani 1 1 d . . .
P1 P 0.69434(9) 0.47525(11) 0.31486(11) 0.0244(3) Uani 1 1 d . . .
P2 P 0.54656(9) 0.63900(10) 0.33272(10) 0.0206(3) Uani 1 1 d . . .
Cl1 Cl 0.57583(10) 0.30624(10) 0.43586(10) 0.0298(3) Uani 1 1 d . . .
Cl2 Cl 0.47162(9) 0.42985(10) 0.25302(10) 0.0271(3) Uani 1 1 d . . .
Cl3 Cl 0.39887(9) 0.46982(10) 0.46535(9) 0.0242(3) Uani 1 1 d . . .
C1 C 0.7277(4) 0.3713(5) 0.2585(5) 0.0382(17) Uani 1 1 d . . .
H1A H 0.7335 0.3195 0.2984 0.057 Uiso 1 1 calc R . .
H1B H 0.7828 0.3828 0.2309 0.057 Uiso 1 1 calc R . .
H1C H 0.6847 0.3555 0.2158 0.057 Uiso 1 1 calc R . .
C2 C 0.7845(4) 0.5063(6) 0.3817(5) 0.0358(16) Uani 1 1 d . . .
H2A H 0.7704 0.5624 0.4142 0.054 Uiso 1 1 calc R . .
H2B H 0.8349 0.5185 0.3464 0.054 Uiso 1 1 calc R . .
H2C H 0.7969 0.4548 0.4205 0.054 Uiso 1 1 calc R . .
C3 C 0.6852(4) 0.5682(4) 0.2365(4) 0.0216(12) Uani 1 1 d . . .
C4 C 0.7429(4) 0.5714(4) 0.1691(4) 0.0275(13) Uani 1 1 d . . .
H4 H 0.7872 0.5262 0.1650 0.033 Uiso 1 1 calc R . .
C5 C 0.7357(4) 0.6406(4) 0.1079(4) 0.0281(14) Uani 1 1 d . . .
H5 H 0.7748 0.6424 0.0620 0.034 Uiso 1 1 calc R . .
C6 C 0.6717(4) 0.7065(5) 0.1141(4) 0.0301(14) Uani 1 1 d . . .
H6 H 0.6671 0.7542 0.0728 0.036 Uiso 1 1 calc R . .
C7 C 0.6139(4) 0.7033(4) 0.1805(4) 0.0258(13) Uani 1 1 d . . .
H7 H 0.5693 0.7482 0.1833 0.031 Uiso 1 1 calc R . .
C8 C 0.6200(3) 0.6353(4) 0.2435(4) 0.0205(12) Uani 1 1 d . . .
C9 C 0.4464(4) 0.6862(4) 0.2943(5) 0.0310(15) Uani 1 1 d . . .
H9A H 0.4184 0.6403 0.2577 0.046 Uiso 1 1 calc R . .
H9B H 0.4575 0.7433 0.2621 0.046 Uiso 1 1 calc R . .
H9C H 0.4089 0.7005 0.3422 0.046 Uiso 1 1 calc R . .
C10 C 0.5916(4) 0.7293(4) 0.3988(4) 0.0302(14) Uani 1 1 d . . .
H10A H 0.5563 0.7368 0.4495 0.045 Uiso 1 1 calc R . .
H10B H 0.5931 0.7882 0.3674 0.045 Uiso 1 1 calc R . .
H10C H 0.6500 0.7119 0.4153 0.045 Uiso 1 1 calc R . .
Cl4 Cl -0.0997(5) 0.5987(5) 0.5524(5) 0.0288(16) Uiso 0.20 1 d PD . .
Cl5 Cl 0.0303(7) 0.4941(9) 0.4594(8) 0.064(3) Uiso 0.20 1 d PD . .
Cl6 Cl -0.0588(7) 0.5719(7) 0.5313(8) 0.060(3) Uiso 0.20 1 d PD . .
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'
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'
In In -0.7276 1.3100 '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
Cl1 In1 Cl2 100.06(5) . . ?
Cl1 In1 Cl3 93.63(5) . . ?
Cl2 In1 Cl3 90.86(5) . . ?
Cl1 In1 P1 90.53(5) . . ?
Cl2 In1 P1 92.01(5) . . ?
Cl3 In1 P1 174.46(5) . . ?
Cl1 In1 Cl3 89.64(5) . 5_666 ?
Cl2 In1 Cl3 168.70(5) . 5_666 ?
Cl3 In1 Cl3 82.70(5) . 5_666 ?
P1 In1 Cl3 93.69(5) . 5_666 ?
Cl1 In1 P2 167.24(5) . . ?
Cl2 In1 P2 84.67(5) . . ?
Cl3 In1 P2 98.16(5) . . ?
P1 In1 P2 77.40(5) . . ?
Cl3 In1 P2 87.05(5) 5_666 . ?
C1 P1 C2 105.4(3) . . ?
C1 P1 C3 106.7(3) . . ?
C2 P1 C3 106.1(3) . . ?
C1 P1 In1 115.2(2) . . ?
C2 P1 In1 116.7(2) . . ?
C3 P1 In1 106.00(19) . . ?
C10 P2 C9 105.3(3) . . ?
C10 P2 C8 103.0(3) . . ?
C9 P2 C8 107.1(3) . . ?
C10 P2 In1 119.3(2) . . ?
C9 P2 In1 116.8(2) . . ?
C8 P2 In1 103.92(18) . . ?
In1 Cl3 In1 97.30(5) . 5_666 ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 120.3(5) . . ?
C4 C3 P1 119.5(5) . . ?
C8 C3 P1 120.2(4) . . ?
C5 C4 C3 120.2(6) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 119.9(6) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.2(6) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C8 121.3(6) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C3 118.1(5) . . ?
C7 C8 P2 119.4(4) . . ?
C3 C8 P2 122.5(4) . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 C10 H10A 109.5 . . ?
P2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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
In1 Cl1 2.4389(15) . ?
In1 Cl2 2.4736(16) . ?
In1 Cl3 2.5721(14) . ?
In1 P1 2.6278(16) . ?
In1 Cl3 2.6555(15) 5_666 ?
In1 P2 2.6575(15) . ?
P1 C1 1.813(7) . ?
P1 C2 1.817(7) . ?
P1 C3 1.826(6) . ?
P2 C10 1.808(6) . ?
P2 C9 1.810(6) . ?
P2 C8 1.821(6) . ?
Cl3 In1 2.6555(15) 5_666 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.398(8) . ?
C3 C8 1.406(8) . ?
C4 C5 1.391(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(8) . ?
C7 H7 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
