#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:44:23 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178627 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/38/4073863.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_4073863
loop_
_publ_author_name
'Han, Ying-Feng'
'Lin, Yue-Jian'
'Jia, Wei-Guo'
'Weng, Lin-Hong'
'Jin, Guo-Xin'
_publ_section_title
;
 Stepwise Formation of Tetra- and Hexanuclear Iridium and Rhodium
 Complexes Containing Oxalato Ligands
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5848
_journal_paper_doi               10.1021/om700691u
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C22 H30 Cl2 O4 Rh2'
_chemical_formula_weight         635.18
_chemical_name_systematic
; 
 ? 
;
_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                 93.999(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.387(3)
_cell_length_b                   8.827(3)
_cell_length_c                   16.629(6)
_cell_measurement_reflns_used    822
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.967
_cell_measurement_theta_min      2.614
_cell_volume                     1228.1(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5963
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        4.09
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.9540
_exptl_absorpt_correction_T_min  0.8836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0422
_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)+(0.0513P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                2151
_reflns_number_total             2687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700691u-file001.cif
_cod_data_source_block           f61220b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1228.1(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4073863
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 0.73260(4) 0.91418(4) 0.11798(2) 0.03375(13) Uani 1 1 d .
Cl1 Cl 0.76678(18) 1.17951(15) 0.13897(10) 0.0636(4) Uani 1 1 d .
O1 O 0.4811(4) 0.9537(4) 0.10068(19) 0.0440(8) Uani 1 1 d .
O2 O 0.7016(3) 0.9592(4) -0.00863(19) 0.0436(8) Uani 1 1 d .
C1 C 0.4363(5) 0.9989(5) 0.0315(3) 0.0355(9) Uani 1 1 d .
C2 C 0.7655(6) 0.6772(6) 0.1181(3) 0.0499(13) Uani 1 1 d .
C3 C 0.9151(5) 0.7510(6) 0.1087(3) 0.0456(11) Uani 1 1 d .
C4 C 0.9535(5) 0.8425(6) 0.1760(3) 0.0439(11) Uani 1 1 d .
C5 C 0.8294(6) 0.8296(6) 0.2299(3) 0.0492(13) Uani 1 1 d .
C6 C 0.7131(6) 0.7262(6) 0.1950(3) 0.0566(15) Uani 1 1 d .
C7 C 0.6801(10) 0.5682(7) 0.0611(5) 0.107(3) Uani 1 1 d .
H7A H 0.6990 0.5952 0.0067 0.161 Uiso 1 1 calc R
H7B H 0.5675 0.5719 0.0681 0.161 Uiso 1 1 calc R
H7C H 0.7190 0.4675 0.0721 0.161 Uiso 1 1 calc R
C8 C 1.0113(8) 0.7384(8) 0.0375(4) 0.084(2) Uani 1 1 d .
H8A H 1.0622 0.8337 0.0283 0.126 Uiso 1 1 calc R
H8B H 0.9427 0.7120 -0.0091 0.126 Uiso 1 1 calc R
H8C H 1.0911 0.6614 0.0470 0.126 Uiso 1 1 calc R
C9 C 1.1017(7) 0.9340(7) 0.1895(4) 0.0758(19) Uani 1 1 d .
H9A H 1.1760 0.8816 0.2262 0.114 Uiso 1 1 calc R
H9B H 1.0761 1.0305 0.2120 0.114 Uiso 1 1 calc R
H9C H 1.1487 0.9490 0.1391 0.114 Uiso 1 1 calc R
C10 C 0.8285(10) 0.9040(9) 0.3098(4) 0.097(3) Uani 1 1 d .
H10A H 0.9219 0.8742 0.3427 0.145 Uiso 1 1 calc R
H10B H 0.7345 0.8740 0.3356 0.145 Uiso 1 1 calc R
H10C H 0.8284 1.0120 0.3030 0.145 Uiso 1 1 calc R
C11 C 0.5627(7) 0.6810(10) 0.2301(5) 0.110(3) Uani 1 1 d .
H11A H 0.5748 0.5815 0.2530 0.165 Uiso 1 1 calc R
H11B H 0.4771 0.6804 0.1886 0.165 Uiso 1 1 calc R
H11C H 0.5386 0.7518 0.2713 0.165 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'
Rh Rh -1.1178 0.9187 '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'
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
C6 Rh1 C2 40.1(2) . .
C6 Rh1 C5 39.6(2) . .
C2 Rh1 C5 66.86(19) . .
C6 Rh1 C3 66.18(19) . .
C2 Rh1 C3 39.63(19) . .
C5 Rh1 C3 65.69(18) . .
C6 Rh1 C4 65.94(18) . .
C2 Rh1 C4 66.10(19) . .
C5 Rh1 C4 39.26(19) . .
C3 Rh1 C4 38.57(18) . .
C6 Rh1 O1 95.30(15) . .
C2 Rh1 O1 106.84(17) . .
C5 Rh1 O1 119.41(17) . .
C3 Rh1 O1 144.45(17) . .
C4 Rh1 O1 158.55(16) . .
C6 Rh1 O2 137.2(2) . .
C2 Rh1 O2 101.05(17) . .
C5 Rh1 O2 160.77(16) . .
C3 Rh1 O2 95.35(15) . .
C4 Rh1 O2 122.98(15) . .
O1 Rh1 O2 77.66(11) . .
C6 Rh1 Cl1 134.26(18) . .
C2 Rh1 Cl1 163.78(14) . .
C5 Rh1 Cl1 100.57(16) . .
C3 Rh1 Cl1 126.86(15) . .
C4 Rh1 Cl1 97.69(15) . .
O1 Rh1 Cl1 88.09(10) . .
O2 Rh1 Cl1 88.10(10) . .
C1 O1 Rh1 114.0(3) . .
C1 O2 Rh1 113.6(3) 3_675 .
O2 C1 O1 125.9(4) 3_675 .
O2 C1 C1 117.4(5) 3_675 3_675
O1 C1 C1 116.7(5) . 3_675
C3 C2 C6 106.4(4) . .
C3 C2 C7 127.4(6) . .
C6 C2 C7 126.1(6) . .
C3 C2 Rh1 70.4(3) . .
C6 C2 Rh1 69.9(3) . .
C7 C2 Rh1 125.5(4) . .
C4 C3 C2 109.3(4) . .
C4 C3 C8 125.1(5) . .
C2 C3 C8 125.6(5) . .
C4 C3 Rh1 71.1(3) . .
C2 C3 Rh1 70.0(3) . .
C8 C3 Rh1 123.1(4) . .
C3 C4 C5 108.6(4) . .
C3 C4 C9 125.3(5) . .
C5 C4 C9 126.1(5) . .
C3 C4 Rh1 70.3(3) . .
C5 C4 Rh1 69.9(3) . .
C9 C4 Rh1 126.9(4) . .
C4 C5 C6 107.7(4) . .
C4 C5 C10 125.3(6) . .
C6 C5 C10 126.9(6) . .
C4 C5 Rh1 70.8(3) . .
C6 C5 Rh1 70.1(3) . .
C10 C5 Rh1 127.4(4) . .
C5 C6 C2 108.0(4) . .
C5 C6 C11 126.1(6) . .
C2 C6 C11 125.9(6) . .
C5 C6 Rh1 70.4(3) . .
C2 C6 Rh1 69.9(3) . .
C11 C6 Rh1 123.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C6 2.110(5) .
Rh1 C2 2.110(5) .
Rh1 C5 2.114(4) .
Rh1 C3 2.115(4) .
Rh1 C4 2.125(4) .
Rh1 O1 2.138(3) .
Rh1 O2 2.141(3) .
Rh1 Cl1 2.3823(16) .
O1 C1 1.251(5) .
O2 C1 1.248(5) 3_675
C1 O2 1.248(5) 3_675
C1 C1 1.547(8) 3_675
C2 C3 1.432(7) .
C2 C6 1.448(7) .
C2 C7 1.497(8) .
C3 C4 1.400(7) .
C3 C8 1.483(6) .
C4 C5 1.424(7) .
C4 C9 1.486(7) .
C5 C6 1.429(8) .
C5 C10 1.484(7) .
C6 C11 1.480(7) .
