#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/84/2208420.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_2208420
loop_
_publ_author_name
'Batsanov, Andrei S.'
'Marder, Todd B.'
'Seeler, Fabian'
_publ_section_title
;fac-Dichlorotris(trimethylphosphine)(trimethylphosphoniomethyl)rhodium(III)
 chloride/bromide dichloromethane benzene solvate
;
_journal_coeditor_code           SG2004
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m574
_journal_page_last               m575
_journal_paper_doi               10.1107/S1600536806005630
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[Rh Cl2 (C4 H11 P) (C3 H9 P)3] (Br0.12/Cl0.88), C H2 Cl2, C6 H6'
_chemical_formula_moiety
'C13 H38 Cl2 P4 Rh +, 0.88 Cl -,0.12 Br -, C6 H6, C H2 Cl2'
_chemical_formula_sum            'C20 H46 Br0.125 Cl4.875 P4 Rh'
_chemical_formula_weight         696.17
_chemical_name_systematic
;
fac-Dichlorotris(trimethylphosphine)(trimethylphosphoniomethyl)rhodium(I)
chloride/bromide benzene dichloromethane solvate
;
_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_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.949(3)
_cell_length_b                   10.3396(15)
_cell_length_c                   18.424(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.73
_cell_measurement_theta_min      12.08
_cell_volume                     3117.7(9)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART 6K CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55018
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.8451
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1433
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.817
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         13203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0339P)²+0.4573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                10300
_reflns_number_total             13203
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sg2004.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208420
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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
Rh Rh 0.229827(6) 0.536706(10) 0.289944(6) 0.01384(3) Uani d . 1 . .
Cl Cl1 0.18701(2) 0.61106(3) 0.159669(19) 0.02219(7) Uani d . 1 . .
Cl Cl2 0.14223(2) 0.70624(4) 0.31903(2) 0.02406(7) Uani d . 1 . .
P P1 0.33377(2) 0.81314(4) 0.25532(2) 0.01798(7) Uani d . 1 . .
P P2 0.30304(2) 0.38566(3) 0.24615(2) 0.01641(7) Uani d . 1 . .
P P3 0.28405(2) 0.48700(4) 0.41363(2) 0.01699(7) Uani d . 1 . .
P P4 0.11282(2) 0.40051(4) 0.27184(2) 0.01937(7) Uani d . 1 . .
C C1 0.32553(8) 0.67881(13) 0.31290(8) 0.0166(2) Uani d . 1 . .
H H11 0.3264 0.7153 0.3628 0.022 Uiso d R 1 . .
H H12 0.3771 0.6298 0.3197 0.022 Uiso d R 1 . .
C C2 0.37100(11) 0.77446(16) 0.17549(9) 0.0272(3) Uani d . 1 . .
H H21 0.4211 0.7232 0.1917 0.033(3) Uiso d R 1 . .
H H22 0.3827 0.8545 0.1517 0.033(3) Uiso d R 1 . .
H H23 0.3296 0.7245 0.1393 0.033(3) Uiso d R 1 . .
C C3 0.41169(9) 0.91431(14) 0.31234(9) 0.0220(3) Uani d . 1 . .
H H31 0.3916 0.9528 0.3527 0.033(3) Uiso d R 1 . .
H H32 0.4256 0.9831 0.2812 0.033(3) Uiso d R 1 . .
H H33 0.4604 0.8623 0.3342 0.033(3) Uiso d R 1 . .
C C4 0.24409(10) 0.91192(15) 0.22570(10) 0.0282(3) Uani d . 1 . .
H H41 0.2003 0.8618 0.1923 0.037(3) Uiso d R 1 . .
H H42 0.2565 0.9879 0.1988 0.037(3) Uiso d R 1 . .
H H43 0.2265 0.9400 0.2698 0.037(3) Uiso d R 1 . .
C C5 0.25121(10) 0.31665(16) 0.15535(9) 0.0256(3) Uani d . 1 . .
H H51 0.2419 0.3844 0.1169 0.048(4) Uiso d R 1 . .
H H52 0.1987 0.2801 0.1580 0.048(4) Uiso d R 1 . .
H H53 0.2852 0.2483 0.1423 0.048(4) Uiso d R 1 . .
C C6 0.39691(10) 0.44019(16) 0.22732(11) 0.0285(3) Uani d . 1 . .
H H61 0.4214 0.3692 0.2055 0.035(3) Uiso d R 1 . .
H H62 0.4350 0.4682 0.2743 0.035(3) Uiso d R 1 . .
H H63 0.3853 0.5128 0.1919 0.035(3) Uiso d R 1 . .
C C7 0.33736(11) 0.23993(15) 0.30053(9) 0.0275(3) Uani d . 1 . .
H H71 0.3673 0.1850 0.2734 0.036(3) Uiso d R 1 . .
H H72 0.2899 0.1927 0.3079 0.036(3) Uiso d R 1 . .
H H73 0.3734 0.2636 0.3495 0.036(3) Uiso d R 1 . .
C C8 0.25986(11) 0.33373(16) 0.45108(9) 0.0273(3) Uani d . 1 . .
H H81 0.2899 0.3267 0.5041 0.037(3) Uiso d R 1 . .
H H82 0.2756 0.2625 0.4227 0.037(3) Uiso d R 1 . .
H H83 0.2010 0.3294 0.4466 0.037(3) Uiso d R 1 . .
C C9 0.39542(9) 0.49043(17) 0.44665(9) 0.0245(3) Uani d . 1 . .
H H91 0.4147 0.5797 0.4461 0.034(3) Uiso d R 1 . .
H H92 0.4189 0.4371 0.4135 0.034(3) Uiso d R 1 . .
H H93 0.4124 0.4564 0.4980 0.034(3) Uiso d R 1 . .
C C10 0.25548(11) 0.59942(17) 0.47770(9) 0.0287(3) Uani d . 1 . .
H H101 0.1961 0.5974 0.4702 0.043(4) Uiso d R 1 . .
H H102 0.2725 0.6869 0.4680 0.043(4) Uiso d R 1 . .
H H103 0.2824 0.5747 0.5296 0.043(4) Uiso d R 1 . .
C C11 0.04928(10) 0.42890(19) 0.33590(10) 0.0310(4) Uani d . 1 . .
H H111 0.0325 0.5199 0.3330 0.049(4) Uiso d R 1 . .
H H112 0.0804 0.4086 0.3873 0.049(4) Uiso d R 1 . .
H H113 0.0007 0.3736 0.3219 0.049(4) Uiso d R 1 . .
C C12 0.11822(11) 0.22318(16) 0.27556(10) 0.0304(4) Uani d . 1 . .
H H121 0.0628 0.1874 0.2635 0.044(4) Uiso d R 1 . .
H H122 0.1481 0.1957 0.3262 0.044(4) Uiso d R 1 . .
H H123 0.1467 0.1918 0.2390 0.044(4) Uiso d R 1 . .
C C13 0.04018(10) 0.4277(2) 0.18184(10) 0.0325(4) Uani d . 1 . .
H H131 -0.0084 0.3741 0.1782 0.044(4) Uiso d R 1 . .
H H132 0.0653 0.4045 0.1413 0.044(4) Uiso d R 1 . .
H H133 0.0244 0.5191 0.1773 0.044(4) Uiso d R 1 . .
Cl Cl3 0.42954(2) 0.11637(3) 0.144351(17) 0.02349(6) Uani d P 0.88 A 1
Br Br3 0.42954(2) 0.11637(3) 0.144351(17) 0.02349(6) Uani d P 0.12 B 2
Cl Cl4 0.09222(3) 0.41111(5) -0.03212(3) 0.03798(10) Uani d . 1 . .
Cl Cl5 0.24553(3) 0.52306(5) -0.04391(4) 0.05161(15) Uani d . 1 . .
C C14 0.14745(12) 0.55584(18) -0.03378(10) 0.0332(4) Uani d . 1 . .
H H141 0.1520 0.6042 0.0135 0.043 Uiso d R 1 . .
H H142 0.1175 0.6107 -0.0761 0.043 Uiso d R 1 . .
C C15 0.50603(17) 0.6315(2) 0.00684(14) 0.0600(8) Uani d . 1 . .
H H15 0.5097 0.7230 0.0113 0.072 Uiso d R 1 . .
C C16 0.44929(14) 0.5659(3) 0.03177(12) 0.0529(7) Uani d . 1 . .
H H16 0.4139 0.6124 0.0547 0.063 Uiso d R 1 . .
C C17 0.44154(14) 0.4357(3) 0.02495(13) 0.0558(7) Uani d . 1 . .
H H17 0.4005 0.3916 0.0419 0.067 Uiso d R 1 . .
C C18 0.01271(16) 0.1256(2) 0.02329(13) 0.0475(6) Uani d . 1 . .
H H18 0.0213 0.2127 0.0399 0.057 Uiso d R 1 . .
C C19 0.07078(13) 0.0337(2) 0.05252(12) 0.0437(5) Uani d . 1 . .
H H19 0.1198 0.0577 0.0884 0.052 Uiso d R 1 . .
C C20 0.05787(14) -0.0927(2) 0.02988(13) 0.0457(5) Uani d . 1 . .
H H20 0.0974 -0.1569 0.0507 0.055 Uiso d R 1 . .
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C1 Rh P2 . . 94.94(4)
C1 Rh P3 . . 82.53(4)
P2 Rh P3 . . 94.848(17)
C1 Rh P4 . . 171.86(4)
P2 Rh P4 . . 93.191(18)
P3 Rh P4 . . 96.375(16)
C1 Rh Cl1 . . 89.68(4)
P2 Rh Cl1 . . 85.269(16)
P3 Rh Cl1 . . 172.191(14)
P4 Rh Cl1 . . 91.412(16)
C1 Rh Cl2 . . 86.38(4)
P2 Rh Cl2 . . 172.141(14)
P3 Rh Cl2 . . 93.005(16)
P4 Rh Cl2 . . 85.625(18)
Cl1 Rh Cl2 . . 86.992(16)
C1 P1 C2 . . 114.56(7)
C1 P1 C4 . . 115.79(8)
C2 P1 C4 . . 109.20(9)
C1 P1 C3 . . 105.46(7)
C2 P1 C3 . . 104.37(8)
C4 P1 C3 . . 106.41(8)
C6 P2 C7 . . 101.13(8)
C6 P2 C5 . . 100.64(8)
C7 P2 C5 . . 100.96(8)
C6 P2 Rh . . 116.37(6)
C7 P2 Rh . . 120.02(6)
C5 P2 Rh . . 114.74(5)
C10 P3 C8 . . 100.80(8)
C10 P3 C9 . . 101.47(8)
C8 P3 C9 . . 101.90(8)
C10 P3 Rh . . 113.57(6)
C8 P3 Rh . . 120.21(6)
C9 P3 Rh . . 116.16(5)
C13 P4 C11 . . 101.13(9)
C13 P4 C12 . . 101.79(9)
C11 P4 C12 . . 99.75(9)
C13 P4 Rh . . 112.28(6)
C11 P4 Rh . . 115.20(6)
C12 P4 Rh . . 123.57(6)
P1 C1 Rh . . 126.18(7)
P1 C1 H11 . . 105.8
Rh C1 H11 . . 105.8
P1 C1 H12 . . 105.8
Rh C1 H12 . . 105.8
H11 C1 H12 . . 106.2
P1 C2 H21 . . 109.5
P1 C2 H22 . . 109.5
H21 C2 H22 . . 109.5
P1 C2 H23 . . 109.5
H21 C2 H23 . . 109.5
H22 C2 H23 . . 109.5
P1 C3 H31 . . 109.5
P1 C3 H32 . . 109.5
H31 C3 H32 . . 109.5
P1 C3 H33 . . 109.5
H31 C3 H33 . . 109.5
H32 C3 H33 . . 109.5
P1 C4 H41 . . 109.5
P1 C4 H42 . . 109.5
H41 C4 H42 . . 109.5
P1 C4 H43 . . 109.5
H41 C4 H43 . . 109.5
H42 C4 H43 . . 109.5
P2 C5 H51 . . 109.5
P2 C5 H52 . . 109.5
H51 C5 H52 . . 109.5
P2 C5 H53 . . 109.5
H51 C5 H53 . . 109.5
H52 C5 H53 . . 109.5
P2 C6 H61 . . 109.5
P2 C6 H62 . . 109.5
H61 C6 H62 . . 109.5
P2 C6 H63 . . 109.5
H61 C6 H63 . . 109.5
H62 C6 H63 . . 109.5
P2 C7 H71 . . 109.5
P2 C7 H72 . . 109.5
H71 C7 H72 . . 109.5
P2 C7 H73 . . 109.5
H71 C7 H73 . . 109.5
H72 C7 H73 . . 109.5
P3 C8 H81 . . 109.5
P3 C8 H82 . . 109.5
H81 C8 H82 . . 109.5
P3 C8 H83 . . 109.5
H81 C8 H83 . . 109.5
H82 C8 H83 . . 109.5
P3 C9 H91 . . 109.5
P3 C9 H92 . . 109.5
H91 C9 H92 . . 109.5
P3 C9 H93 . . 109.5
H91 C9 H93 . . 109.5
H92 C9 H93 . . 109.5
P3 C10 H101 . . 109.5
P3 C10 H102 . . 109.5
H101 C10 H102 . . 109.5
P3 C10 H103 . . 109.5
H101 C10 H103 . . 109.5
H102 C10 H103 . . 109.5
P4 C11 H111 . . 109.5
P4 C11 H112 . . 109.5
H111 C11 H112 . . 109.5
P4 C11 H113 . . 109.5
H111 C11 H113 . . 109.5
H112 C11 H113 . . 109.5
P4 C12 H121 . . 109.5
P4 C12 H122 . . 109.5
H121 C12 H122 . . 109.5
P4 C12 H123 . . 109.5
H121 C12 H123 . . 109.5
H122 C12 H123 . . 109.5
P4 C13 H131 . . 109.5
P4 C13 H132 . . 109.5
H131 C13 H132 . . 109.5
P4 C13 H133 . . 109.5
H131 C13 H133 . . 109.5
H132 C13 H133 . . 109.5
Cl5 C14 Cl4 . . 111.03(10)
Cl5 C14 H141 . . 109.4
Cl4 C14 H141 . . 109.4
Cl5 C14 H142 . . 109.4
Cl4 C14 H142 . . 109.5
H141 C14 H142 . . 108.0
C16 C15 C17 . 3_665 119.2(2)
C16 C15 H15 . . 120.4
C17 C15 H15 3_665 . 120.4
C15 C16 C17 . . 121.8(2)
C15 C16 H16 . . 119.1
C17 C16 H16 . . 119.1
C16 C17 C15 . 3_665 119.0(2)
C16 C17 H17 . . 120.5
C15 C17 H17 3_665 . 120.5
C19 C18 C20 . 3 120.6(2)
C19 C18 H18 . . 119.7
C20 C18 H18 3 . 119.7
C20 C19 C18 . . 119.9(2)
C20 C19 H19 . . 120.1
C18 C19 H19 . . 120.0
C19 C20 C18 . 3 119.5(2)
C19 C20 H20 . . 120.2
C18 C20 H20 3 . 120.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Rh C1 . 2.1475(14)
Rh P2 . 2.2695(4)
Rh P3 . 2.2832(5)
Rh P4 . 2.3840(5)
Rh Cl1 . 2.4439(5)
Rh Cl2 . 2.4449(4)
P1 C1 . 1.7751(14)
P1 C2 . 1.7900(16)
P1 C4 . 1.7944(16)
P1 C3 . 1.7946(15)
P2 C6 . 1.8046(16)
P2 C7 . 1.8191(16)
P2 C5 . 1.8208(16)
P3 C10 . 1.8100(17)
P3 C8 . 1.8174(16)
P3 C9 . 1.8267(16)
P4 C13 . 1.8117(17)
P4 C11 . 1.8165(17)
P4 C12 . 1.8362(18)
C1 H11 . 0.9900
C1 H12 . 0.9900
C2 H21 . 0.9800
C2 H22 . 0.9801
C2 H23 . 0.9799
C3 H31 . 0.9799
C3 H32 . 0.9800
C3 H33 . 0.9799
C4 H41 . 0.9799
C4 H42 . 0.9800
C4 H43 . 0.9799
C5 H51 . 0.9799
C5 H52 . 0.9800
C5 H53 . 0.9800
C6 H61 . 0.9799
C6 H62 . 0.9800
C6 H63 . 0.9800
C7 H71 . 0.9800
C7 H72 . 0.9799
C7 H73 . 0.9799
C8 H81 . 0.9800
C8 H82 . 0.9800
C8 H83 . 0.9801
C9 H91 . 0.9800
C9 H92 . 0.9800
C9 H93 . 0.9799
C10 H101 . 0.9801
C10 H102 . 0.9799
C10 H103 . 0.9801
C11 H111 . 0.9800
C11 H112 . 0.9800
C11 H113 . 0.9800
C12 H121 . 0.9800
C12 H122 . 0.9800
C12 H123 . 0.9799
C13 H131 . 0.9799
C13 H132 . 0.9800
C13 H133 . 0.9800
Cl4 C14 . 1.770(2)
Cl5 C14 . 1.753(2)
C14 H141 . 0.9900
C14 H142 . 0.9900
C15 C16 . 1.351(4)
C15 C17 3_665 1.373(4)
C15 H15 . 0.9500
C16 C17 . 1.356(4)
C16 H16 . 0.9499
C17 C15 3_665 1.373(4)
C17 H17 . 0.9499
C18 C19 . 1.373(3)
C18 C20 3 1.377(3)
C18 H18 . 0.9500
C19 C20 . 1.372(3)
C19 H19 . 0.9500
C20 C18 3 1.378(3)
C20 H20 . 0.9499
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C14 H141 Cl1 . 0.99 2.60 3.498(2) 150
C14 H142 Cl2 4_575 0.99 2.81 3.6455(19) 142
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
Cl1 Rh C1 P1 14.80(9)
Rh C1 P1 C3 167.66(9)
