#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/28/2232893.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_2232893
loop_
_publ_author_name
'Warsink, Stefan'
'Koen, Renier'
'Roodt, Andreas'
_publ_section_title
;
 trans-Carbonylchloridobis(tri-o-tolylphosphane-κP)rhodium(I)
;
_journal_coeditor_code           PV2465
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1666
_journal_paper_doi               10.1107/S1600536811045715
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Rh Cl (C21 H21 P)2 (C O)]'
_chemical_formula_moiety         'C43 H42 Cl O P2 Rh'
_chemical_formula_sum            'C43 H42 Cl O P2 Rh'
_chemical_formula_weight         775.07
_chemical_name_systematic
;
trans-Carbonylchloridobis(tri-o-tolylphosphane-
κP)rhodium(I)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 93.102(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   10.6440(14)
_cell_length_b                   10.9464(15)
_cell_length_c                   15.605(2)
_cell_measurement_reflns_used    6713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.27
_cell_volume                     1815.5(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2007)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8 APEXII 4K KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21616
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.123
_refine_diff_density_max         2.352
_refine_diff_density_min         -1.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0845P)²+0.2003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                3344
_reflns_number_total             4481
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pv2465.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2232893
_cod_database_fobs_code          2232893
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
C C1 0.1009(10) -0.1237(10) 0.4794(7) 0.025(2) Uani d P 0.50 1
C C2 0.2646(3) 0.1270(3) 0.4195(2) 0.0193(7) Uani d . 1 1
C C3 0.3138(3) 0.1696(3) 0.4992(2) 0.0249(8) Uani d . 1 1
C C4 0.4438(4) 0.1739(3) 0.5146(3) 0.0294(8) Uani d . 1 1
H H10 0.4765 0.2061 0.5663 0.035 Uiso calc R 1 1
C C5 0.5256(4) 0.1321(3) 0.4558(3) 0.0312(9) Uani d . 1 1
H H6 0.6121 0.1359 0.4676 0.037 Uiso calc R 1 1
C C6 0.4771(3) 0.0841(3) 0.3786(2) 0.0279(8) Uani d . 1 1
H H15 0.5311 0.0537 0.3389 0.033 Uiso calc R 1 1
C C7 0.3484(3) 0.0814(3) 0.3608(2) 0.0230(7) Uani d . 1 1
H H9 0.3168 0.0488 0.3090 0.028 Uiso calc R 1 1
C C8 0.2326(4) 0.2095(4) 0.5707(2) 0.0345(9) Uani d . 1 1
H H24A 0.1527 0.2374 0.5467 0.052 Uiso calc R 1 1
H H24B 0.2736 0.2747 0.6024 0.052 Uiso calc R 1 1
H H24C 0.2198 0.1418 0.6083 0.052 Uiso calc R 1 1
C C9 0.0342(3) 0.2733(3) 0.3794(2) 0.0211(7) Uani d . 1 1
C C10 0.1102(4) 0.3733(3) 0.4027(2) 0.0263(8) Uani d . 1 1
H H22 0.1910 0.3603 0.4266 0.032 Uiso calc R 1 1
C C11 0.0664(4) 0.4919(3) 0.3905(3) 0.0327(9) Uani d . 1 1
H H18 0.1174 0.5581 0.4062 0.039 Uiso calc R 1 1
C C12 -0.0537(4) 0.5105(3) 0.3547(3) 0.0362(10) Uani d . 1 1
H H4 -0.0836 0.5897 0.3462 0.043 Uiso calc R 1 1
C C13 -0.1299(4) 0.4121(4) 0.3314(3) 0.0319(9) Uani d . 1 1
H H19 -0.2102 0.4264 0.3070 0.038 Uiso calc R 1 1
C C14 -0.0886(3) 0.2918(3) 0.3437(2) 0.0238(7) Uani d . 1 1
C C15 -0.1760(3) 0.1889(4) 0.3142(2) 0.0285(8) Uani d . 1 1
H H14A -0.1528 0.1600 0.2592 0.043 Uiso calc R 1 1
H H14B -0.2611 0.2184 0.3097 0.043 Uiso calc R 1 1
H H14C -0.1695 0.1233 0.3550 0.043 Uiso calc R 1 1
C C16 0.0791(3) 0.0561(3) 0.2837(2) 0.0188(7) Uani d . 1 1
C C17 0.1169(3) 0.1212(3) 0.2114(2) 0.0222(7) Uani d . 1 1
C C18 0.0976(3) 0.0660(4) 0.1308(2) 0.0271(8) Uani d . 1 1
H H23 0.1215 0.1074 0.0822 0.033 Uiso calc R 1 1
C C19 0.0436(4) -0.0488(4) 0.1218(2) 0.0305(8) Uani d . 1 1
H H17 0.0326 -0.0838 0.0676 0.037 Uiso calc R 1 1
C C20 0.0061(3) -0.1115(3) 0.1923(2) 0.0286(8) Uani d . 1 1
H H13 -0.0311 -0.1880 0.1858 0.034 Uiso calc R 1 1
C C21 0.0239(3) -0.0601(3) 0.2729(2) 0.0235(7) Uani d . 1 1
H H5 -0.0008 -0.1029 0.3206 0.028 Uiso calc R 1 1
C C22 0.1748(4) 0.2474(3) 0.2150(2) 0.0273(8) Uani d . 1 1
H H16A 0.2179 0.2619 0.1635 0.041 Uiso calc R 1 1
H H16B 0.2334 0.2529 0.2638 0.041 Uiso calc R 1 1
H H16C 0.1098 0.3073 0.2200 0.041 Uiso calc R 1 1
O O1 0.1652(12) -0.2035(10) 0.4677(9) 0.030(3) Uani d P 0.50 1
P P1 0.09397(8) 0.11591(8) 0.39409(6) 0.0182(2) Uani d . 1 1
Cl Cl1 0.1376(3) -0.1671(3) 0.4666(2) 0.0226(7) Uani d P 0.50 1
Rh Rh1 0.0000 0.0000 0.5000 0.01825(13) Uani d S 1 2
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'
Rh Rh -1.1178 0.9187 '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
Cl1 C1 Rh1 . . 172.6(14)
O1 C1 Rh1 . . 178.8(14)
C3 C2 C7 . . 118.4(3)
C3 C2 P1 . . 122.0(3)
C7 C2 P1 . . 119.3(3)
C4 C3 C2 . . 119.0(3)
C4 C3 C8 . . 117.7(3)
C2 C3 C8 . . 123.3(3)
C5 C4 C3 . . 122.1(4)
C5 C4 H10 . . 119.0
C3 C4 H10 . . 119.0
C4 C5 C6 . . 119.0(3)
C4 C5 H6 . . 120.5
C6 C5 H6 . . 120.5
C7 C6 C5 . . 120.0(4)
C7 C6 H15 . . 120.0
C5 C6 H15 . . 120.0
C6 C7 C2 . . 121.2(3)
C6 C7 H9 . . 119.4
C2 C7 H9 . . 119.4
C3 C8 H24A . . 109.5
C3 C8 H24B . . 109.5
H24A C8 H24B . . 109.5
C3 C8 H24C . . 109.5
H24A C8 H24C . . 109.5
H24B C8 H24C . . 109.5
C10 C9 C14 . . 120.2(3)
C10 C9 P1 . . 120.5(3)
C14 C9 P1 . . 119.3(3)
C11 C10 C9 . . 120.7(4)
C11 C10 H22 . . 119.6
C9 C10 H22 . . 119.6
C12 C11 C10 . . 119.3(4)
C12 C11 H18 . . 120.4
C10 C11 H18 . . 120.4
C11 C12 C13 . . 120.5(4)
C11 C12 H4 . . 119.8
C13 C12 H4 . . 119.8
C12 C13 C14 . . 121.4(4)
C12 C13 H19 . . 119.3
C14 C13 H19 . . 119.3
C13 C14 C9 . . 117.9(3)
C13 C14 C15 . . 118.3(3)
C9 C14 C15 . . 123.7(3)
C14 C15 H14A . . 109.5
C14 C15 H14B . . 109.5
H14A C15 H14B . . 109.5
C14 C15 H14C . . 109.5
H14A C15 H14C . . 109.5
H14B C15 H14C . . 109.5
C21 C16 C17 . . 119.7(3)
C21 C16 P1 . . 116.6(2)
C17 C16 P1 . . 123.7(3)
C18 C17 C16 . . 117.8(3)
C18 C17 C22 . . 117.8(3)
C16 C17 C22 . . 124.4(3)
C19 C18 C17 . . 121.4(3)
C19 C18 H23 . . 119.3
C17 C18 H23 . . 119.3
C20 C19 C18 . . 120.6(3)
C20 C19 H17 . . 119.7
C18 C19 H17 . . 119.7
C19 C20 C21 . . 119.6(4)
C19 C20 H13 . . 120.2
C21 C20 H13 . . 120.2
C20 C21 C16 . . 120.9(3)
C20 C21 H5 . . 119.6
C16 C21 H5 . . 119.6
C17 C22 H16A . . 109.5
C17 C22 H16B . . 109.5
H16A C22 H16B . . 109.5
C17 C22 H16C . . 109.5
H16A C22 H16C . . 109.5
H16B C22 H16C . . 109.5
C16 P1 C2 . . 105.01(15)
C16 P1 C9 . . 101.78(16)
C2 P1 C9 . . 107.12(15)
C16 P1 Rh1 . . 116.59(11)
C2 P1 Rh1 . . 109.66(11)
C9 P1 Rh1 . . 115.72(11)
C1 Rh1 C1 . 3_556 180.000(2)
C1 Rh1 P1 . 3_556 90.0(4)
C1 Rh1 P1 3_556 3_556 90.0(4)
C1 Rh1 P1 . . 90.0(4)
C1 Rh1 P1 3_556 . 90.0(4)
P1 Rh1 P1 3_556 . 180.0
C1 Rh1 Cl1 . . 2.0(4)
C1 Rh1 Cl1 3_556 . 178.0(4)
P1 Rh1 Cl1 3_556 . 91.66(10)
P1 Rh1 Cl1 . . 88.34(10)
C1 Rh1 Cl1 . 3_556 178.0(4)
C1 Rh1 Cl1 3_556 3_556 2.0(4)
P1 Rh1 Cl1 3_556 3_556 88.34(10)
P1 Rh1 Cl1 . 3_556 91.66(10)
Cl1 Rh1 Cl1 . 3_556 180.00(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 Cl1 . 0.654(9)
C1 O1 . 1.131(11)
C1 Rh1 . 1.769(11)
C2 C3 . 1.402(5)
C2 C7 . 1.405(5)
C2 P1 . 1.842(3)
C3 C4 . 1.393(5)
C3 C8 . 1.513(5)
C4 C5 . 1.377(6)
C4 H10 . 0.9300
C5 C6 . 1.387(5)
C5 H6 . 0.9300
C6 C7 . 1.383(5)
C6 H15 . 0.9300
C7 H9 . 0.9300
C8 H24A . 0.9600
C8 H24B . 0.9600
C8 H24C . 0.9600
C9 C10 . 1.398(5)
C9 C14 . 1.407(5)
C9 P1 . 1.846(4)
C10 C11 . 1.389(5)
C10 H22 . 0.9300
C11 C12 . 1.383(7)
C11 H18 . 0.9300
C12 C13 . 1.385(6)
C12 H4 . 0.9300
C13 C14 . 1.399(5)
C13 H19 . 0.9300
C14 C15 . 1.516(5)
C15 H14A . 0.9600
C15 H14B . 0.9600
C15 H14C . 0.9600
C16 C21 . 1.408(5)
C16 C17 . 1.411(5)
C16 P1 . 1.841(3)
C17 C18 . 1.401(5)
C17 C22 . 1.513(5)
C18 C19 . 1.386(6)
C18 H23 . 0.9300
C19 C20 . 1.373(6)
C19 H17 . 0.9300
C20 C21 . 1.382(5)
C20 H13 . 0.9300
C21 H5 . 0.9300
C22 H16A . 0.9600
C22 H16B . 0.9600
C22 H16C . 0.9600
P1 Rh1 . 2.3496(10)
Cl1 Rh1 . 2.418(3)
Rh1 C1 3_556 1.769(11)
Rh1 P1 3_556 2.3496(10)
Rh1 Cl1 3_556 2.418(3)
