#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:44:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178665 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/76/4077664.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_4077664
loop_
_publ_author_name
'Carmona, Daniel'
'Ferrer, Joaquina'
'Arilla, José M.'
'Reyes, Josefa'
'Lahoz, Fernando J.'
'Elipe, Sergio'
'Modrego, F. Javier'
'Oro, Luis A.'
_publ_section_title
;
 Synthesis, Characterization, and Theoretical Studies on Heterobinuclear
 (p-cymene)Os(μ-pz)2M (M = Ir, Rh; Hpz = Pyrazole) Complexes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              798
_journal_paper_doi               10.1021/om990624h
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'C17 H20 I N4 O Os Rh'
_chemical_formula_structural     '[(C10 H14) Os (C3 H3 N2)2 Rh I (C O)]'
_chemical_formula_sum            'C17 H20 I N4 O Os Rh'
_chemical_formula_weight         716.38
_chemical_name_systematic
;
 iodo-carbonyl-(eta$6!-p-cymene)-bis-(mu!2$-pyrazolyl-N,N')-
 rhodium(i)-osmium(ii)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.544(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2213(15)
_cell_length_b                   13.577(2)
_cell_length_c                   16.009(2)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    200.0(2)
_cell_measurement_theta_max      18.5
_cell_measurement_theta_min      12.7
_cell_volume                     1956.4(5)
_computing_cell_refinement       'DIF4 (Stoe)'
_computing_data_collection       'DIF4 (Stoe)'
_computing_data_reduction        'REDU4 (Stoe)'
_computing_molecular_graphics    'XP, SHELXTL v. 5 (Siemens)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200.0(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Siemens-Stoe AED2'
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5803
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.922
_exptl_absorpt_correction_T_max  0.062
_exptl_absorpt_correction_T_min  0.035
_exptl_absorpt_correction_type   '\y scans'
_exptl_absorpt_process_details
;
 Azimuthal psi-scans of 12 reflections at 10° intervals.
 Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0425
_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=3D1/[σ²(Fo²)+(0.0151P)²+0.0000P] where P=3D(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                2381
_reflns_number_total             3438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990624h.cif
_cod_data_source_block           compound12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1956.5(5)
_cod_database_code               4077664
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_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_calc_flag
_atom_site_refinement_flags
Os Os 0.27151(5) 0.12425(3) 0.24181(2) 0.02062(11) Uani 1 d .
Rh Rh 0.17882(9) 0.04694(6) 0.08429(5) 0.0206(2) Uani 1 d .
I I -0.08081(8) -0.02781(5) 0.10219(4) 0.02695(18) Uani 1 d .
N1 N 0.4189(9) 0.1592(6) 0.1655(5) 0.026(2) Uani 1 d .
N2 N 0.3726(8) 0.1178(6) 0.0881(5) 0.0232(19) Uani 1 d .
C1 C 0.5511(12) 0.2040(8) 0.1679(7) 0.034(3) Uani 1 d U
H1 H 0.6218 0.2432 0.2133 0.015(10) Uiso 1 d R
C2 C 0.5889(13) 0.1862(9) 0.0906(7) 0.041(3) Uani 1 d .
H2 H 0.6613 0.2212 0.0785 0.015(10) Uiso 1 d R
C3 C 0.4791(12) 0.1330(9) 0.0429(6) 0.030(3) Uani 1 d U
H3 H 0.4785 0.1131 -0.0155 0.015(10) Uiso 1 d R
N3 N 0.1344(9) 0.2217(6) 0.1634(5) 0.0209(19) Uani 1 d .
N4 N 0.0902(8) 0.1861(6) 0.0824(5) 0.022(2) Uani 1 d .
C4 C 0.0599(11) 0.3058(8) 0.1684(6) 0.028(3) Uani 1 d .
H4 H 0.0568 0.3504 0.2183 0.015(10) Uiso 1 d R
C5 C -0.0285(12) 0.3260(8) 0.0896(6) 0.029(3) Uani 1 d .
H5 H -0.0880 0.3906 0.0571 0.015(10) Uiso 1 d R
C6 C -0.0106(12) 0.2471(8) 0.0382(7) 0.032(3) Uani 1 d .
H6 H -0.0424 0.2496 -0.0179 0.015(10) Uiso 1 d R
C7 C 0.1360(13) 0.1158(10) 0.3385(6) 0.036(3) Uani 1 d U
C8 C 0.1769(12) 0.0213(8) 0.3176(6) 0.025(2) Uani 1 d .
H8 H 0.1049 -0.0226 0.2861 0.017(11) Uiso 1 d R
C9 C 0.3307(11) -0.0067(9) 0.3228(6) 0.028(3) Uani 1 d .
H9 H 0.3234 -0.0749 0.2922 0.017(11) Uiso 1 d R
C10 C 0.4386(12) 0.0619(8) 0.3485(6) 0.028(3) Uani 1 d .
C11 C 0.4016(12) 0.1609(8) 0.3691(6) 0.025(3) Uani 1 d .
H11 H 0.4900 0.2119 0.3702 0.017(11) Uiso 1 d R
C12 C 0.2538(11) 0.1856(9) 0.3659(5) 0.027(3) Uani 1 d .
H12 H 0.2193 0.2628 0.3676 0.017(11) Uiso 1 d R
C13 C -0.0262(11) 0.1461(9) 0.3279(6) 0.035(3) Uani 1 d U
H13A H -0.0865 0.1120 0.2783 0.050(12) Uiso 1 calc R
H13B H -0.0353 0.2174 0.3190 0.050(12) Uiso 1 calc R
H13C H -0.0611 0.1282 0.3795 0.050(12) Uiso 1 calc R
C14 C 0.6028(12) 0.0365(9) 0.3509(6) 0.033(3) Uani 1 d .
H14 H 0.6465 0.1019 0.3443 0.017(11) Uiso 1 d R
C15 C 0.6255(12) -0.0315(9) 0.2786(7) 0.047(3) Uani 1 d .
H15A H 0.5825 -0.0962 0.2852 0.050(12) Uiso 1 calc R
H15B H 0.7320 -0.0386 0.2808 0.050(12) Uiso 1 calc R
H15C H 0.5766 -0.0031 0.2233 0.050(12) Uiso 1 calc R
C16 C 0.6704(15) -0.0061(13) 0.4380(7) 0.075(5) Uani 1 d .
H16A H 0.6220 -0.0688 0.4452 0.050(12) Uiso 1 calc R
H16B H 0.6561 0.0401 0.4826 0.050(12) Uiso 1 calc R
H16C H 0.7769 -0.0170 0.4426 0.050(12) Uiso 1 calc R
C17 C 0.2660(12) -0.0752(9) 0.1108(6) 0.029(3) Uani 1 d U
O1 O 0.3148(9) -0.1487(6) 0.1286(5) 0.039(2) Uani 1 d .
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'
N N 0.0061 0.0033 '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'
Rh Rh -1.1178 0.9187 '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'
Os Os -1.2165 7.6030 '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_3
N3 Os N1 83.5(3) .
N3 Os C8 119.4(4) .
N1 Os C8 151.5(4) .
N3 Os C11 124.2(4) .
N1 Os C11 101.5(4) .
C8 Os C11 80.2(4) .
N3 Os C12 98.7(4) .
N1 Os C12 129.4(4) .
C8 Os C12 67.5(4) .
C11 Os C12 37.1(3) .
N3 Os C7 95.5(4) .
N1 Os C7 167.4(4) .
C8 Os C7 37.5(4) .
C11 Os C7 68.6(4) .
C12 Os C7 38.2(4) .
N3 Os C9 157.0(3) .
N1 Os C9 115.0(4) .
C8 Os C9 39.0(4) .
C11 Os C9 67.6(4) .
C12 Os C9 80.3(4) .
C7 Os C9 69.4(4) .
N3 Os C10 162.2(4) .
N1 Os C10 96.2(4) .
C8 Os C10 67.4(4) .
C11 Os C10 38.4(4) .
C12 Os C10 67.8(4) .
C7 Os C10 81.0(4) .
C9 Os C10 36.0(4) .
N3 Os Rh 69.6(2) .
N1 Os Rh 69.7(2) .
C8 Os Rh 100.9(3) .
C11 Os Rh 163.7(3) .
C12 Os Rh 157.7(3) .
C7 Os Rh 121.8(3) .
C9 Os Rh 103.0(3) .
C10 Os Rh 127.0(3) .
C17 Rh N2 94.7(4) .
C17 Rh N4 167.9(4) .
N2 Rh N4 84.8(3) .
C17 Rh I 89.4(3) .
N2 Rh I 170.2(2) .
N4 Rh I 89.3(2) .
C17 Rh Os 95.8(3) .
N2 Rh Os 71.8(2) .
N4 Rh Os 72.6(2) .
I Rh Os 99.04(3) .
C17 Rh I 100.1(3) 3
N2 Rh I 98.5(2) 3
N4 Rh I 91.9(2) 3
I Rh I 89.45(3) 3
Os Rh I 162.02(4) 3
Rh I Rh 90.55(3) 3
N2 N1 C1 108.6(8) .
N2 N1 Os 109.3(6) .
C1 N1 Os 141.9(7) .
N1 N2 C3 107.9(8) .
N1 N2 Rh 109.2(6) .
C3 N2 Rh 142.7(7) .
N1 C1 C2 107.3(10) .
N1 C1 H1 133.6 .
C2 C1 H1 119.1 .
C3 C2 C1 107.4(10) .
C3 C2 H2 133.2 .
C1 C2 H2 117.3 .
C2 C3 N2 108.8(9) .
C2 C3 H3 122.9 .
N2 C3 H3 128.2 .
C4 N3 N4 107.9(8) .
C4 N3 Os 139.9(7) .
N4 N3 Os 111.7(6) .
C6 N4 N3 108.4(8) .
C6 N4 Rh 144.2(7) .
N3 N4 Rh 106.0(6) .
N3 C4 C5 108.9(9) .
N3 C4 H4 131.3 .
C5 C4 H4 119.7 .
C4 C5 C6 105.5(9) .
C4 C5 H5 136.7 .
C6 C5 H5 116.6 .
N4 C6 C5 109.1(9) .
N4 C6 H6 127.2 .
C5 C6 H6 121.3 .
C8 C7 C12 117.0(10) .
C8 C7 C13 122.0(11) .
C12 C7 C13 121.0(11) .
C8 C7 Os 69.8(6) .
C12 C7 Os 70.9(6) .
C13 C7 Os 127.1(7) .
C7 C8 C9 122.5(10) .
C7 C8 Os 72.7(6) .
C9 C8 Os 72.1(6) .
C7 C8 H8 120.6 .
C9 C8 H8 115.2 .
Os C8 H8 115.4 .
C10 C9 C8 118.7(11) .
C10 C9 Os 72.3(6) .
C8 C9 Os 68.9(6) .
C10 C9 H9 135.9 .
C8 C9 H9 104.1 .
Os C9 H9 117.3 .
C9 C10 C11 120.9(10) .
C9 C10 C14 120.3(10) .
C11 C10 C14 118.8(10) .
C9 C10 Os 71.7(6) .
C11 C10 Os 70.1(6) .
C14 C10 Os 128.4(7) .
C12 C11 C10 119.6(10) .
C12 C11 Os 71.7(5) .
C10 C11 Os 71.6(6) .
C12 C11 H11 125.6 .
C10 C11 H11 113.0 .
Os C11 H11 115.2 .
C11 C12 C7 121.4(11) .
C11 C12 Os 71.2(5) .
C7 C12 Os 70.9(5) .
C11 C12 H12 121.0 .
C7 C12 H12 115.8 .
Os C12 H12 117.7 .
C7 C13 H13A 109.5 .
C7 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
C7 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
C16 C14 C15 111.7(11) .
C16 C14 C10 108.2(9) .
C15 C14 C10 114.2(9) .
C16 C14 H14 110.2 .
C15 C14 H14 109.6 .
C10 C14 H14 102.5 .
C14 C15 H15A 109.5 .
C14 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
C14 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
C14 C16 H16A 109.5 .
C14 C16 H16B 109.5 .
H16A C16 H16B 109.5 .
C14 C16 H16C 109.5 .
H16A C16 H16C 109.5 .
H16B C16 H16C 109.5 .
O1 C17 Rh 177.5(11) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Os N3 2.058(8) .
Os N1 2.070(8) .
Os C8 2.156(10) .
Os C11 2.185(9) .
Os C12 2.192(9) .
Os C7 2.193(10) .
Os C9 2.198(10) .
Os C10 2.206(10) .
Os Rh 2.6936(9) .
Rh C17 1.851(13) .
Rh N2 2.019(8) .
Rh N4 2.056(9) .
Rh I 2.6725(11) .
Rh I 2.9369(10) 3
I Rh 2.9369(10) 3
N1 N2 1.343(10) .
N1 C1 1.355(12) .
N2 C3 1.356(12) .
C1 C2 1.378(14) .
C1 H1 1.0154 .
C2 C3 1.340(14) .
C2 H2 0.8752 .
C3 H3 0.9721 .
N3 C4 1.343(12) .
N3 N4 1.362(10) .
N4 C6 1.328(12) .
C4 C5 1.373(13) .
C4 H4 1.0079 .
C5 C6 1.382(13) .
C5 H5 1.1026 .
C6 H6 0.8830 .
C7 C8 1.398(15) .
C7 C12 1.436(15) .
C7 C13 1.525(14) .
C8 C9 1.453(14) .
C8 H8 0.9510 .
C9 C10 1.360(14) .
C9 H9 1.0428 .
C10 C11 1.443(14) .
C10 C14 1.545(14) .
C11 C12 1.394(13) .
C11 H11 1.0673 .
C12 H12 1.0966 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C16 1.513(14) .
C14 C15 1.530(15) .
C14 H14 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 O1 1.107(13) .
